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    《化學試劑》2022年第2期中英文摘要

    發布時間: 2022-02-21 09:33:26   試劑信息網

    重氮化合物的合成方法

    袁鑫,許家喜*

    北京化工大學 化學學院 有機化學系,北京  100029

     

    摘要:重氮化合物是重要的高活性有機合成中間體,可用來制備烯酮、環丙烷和三元雜環衍生物、環庚三烯衍生物、葉立德、金屬卡賓、和偶氮類化合物等,因此,廣泛應用于有機合成化學、藥物合成化學和農化學品合成,其合成方法和應用都得到了很大發展。目前合成重氮化合物的方法主要分為重氮轉移法、其他官能團的重氮化法和重氮化合物的修飾法3種。對重氮化合物的合成方法,特別是近十余年發展的合成方法進行了綜述,并預測討論了重氮化合物合成今后的發展方向。

    關鍵詞:重氮化合物;重氮轉移;重氮化;衍生化

    中圖分類號:O623.7      文獻標識碼:A      文章編號:0258-3283(2022)--

     

    Synthetic Methods of Diazo Compounds YUAN Xin, XU Jia-xi* (Department of Organic Chemistry, College of Chemistry, Beijing University of Chemical Technology, Beijing 100029, China), Huaxue Shiji, 2022, 44(2), 

    AbstractDiazo compounds are important active organic synthetic intermediates and have been used in preparations of ketenes, cyclopropane and three-membered heterocycle derivatives, cycloheptatriene derivatives, ylides, metaloocarbenes, ketones, and azocompounds, and so on. They have been widely applied in organic synthetic chemistry, pharmaceutical synthetic chemistry, and agrochemical synthesis. Their synthetic methods and applications have been well developed. Three synthetic methods have been developed, including diazo transfer, diazotization of other functional groups, and derivatization of diazo compounds, to date. The synthetic methods, especially new synthetic methods developed in recent decades, of diazo compounds are summarized. New development direction on synthesis of diazo compounds in the future is predicted and discussed.

    Key wordsdiazo compound; diazo transfer; diazotization; derivatization

    引用本文:袁鑫,許家喜. 重氮化合物的合成方法[J]. 化學試劑,2022,44(2):161-168。

     

     

    基于半導體量子點的電致化學發光試劑的研究進展

    張連梅*,王宇紅,趙英杰,劉璐,毛雪,邸萌婕

    (蘭州市疾病預防控制中心 微生物實驗室,甘肅 蘭州  730030)

     

    摘要電致化學發光因為不需要激發光源,沒有雜散光的干擾,實驗設備簡單且具有背景信號低、靈敏度高的優點,近年來在環境監測、食品安全分析、生物傳感和成像等領域都引起了科學家們廣泛地關注。在電致化學發光技術中,發光試劑無疑是最重要的組成部件。隨著納米科學和技術的迅猛發展,半導體量子點由于尺寸調控帶隙、表面易于改性和表面態依賴性的電子轉移、良好的發光強度和單色性而成為一類理想的電致化學發光試劑。首先簡要介紹電致化學發光及其機理,接著重點總結各類半導體量子點的電致化學發光特性,最后對基于半導體量子點的電致化學發光試劑存在的挑戰和機遇進行討論。

    關鍵詞電致化學發光;發光試劑;納米顆粒;半導體量子點

    中圖分類號:O646             文獻標識碼:A             文章編號:0258-32832022

     

    Recent Advances in Semiconductor Quantum Dots as Electrogenerated Chemiluminescence Reagents ZHANG Lian-Mei*, WANG Yu-Hong, ZHAO Ying-Jie, LIU Lu, MAO Xue, DI Meng-Jie (Laboratory of Microbiology, Lanzhou Center for Disease Control and Prevention, Gansu, Lanzhou 730030,China), Huaxue Shiji, 2022, 44(2)

    Abstract: Benefitting from no requirement of excitation light sources, no presence of background emissions from unexpected photoexcitation, simple instruments and apparatus, along with its high sensitivity and low signal-to-noise ratio, electrogenerated chemiluminescence (ECL) has been a superior analytical tool and attracts widespread interests from scientists in the areas of environmental monitoring, food safety analysis, biosensing and bioimaging. With the rapid development of nanoscience and nanotechnology, the novel semiconductor quantum dots (QDs) are affording a new opportunity for exploring ideal nanomaterial based ECL reagents due to their size-regulated band gap, easy surface modification and surface state-dependent electron transfer, excellent emission intensity and monochromaticity. In this review, we firstly provide a brief overview of ECL fundamentals, and then place emphasis on the ECL characteristics of different kinds of semiconductor QDs. The current challenges and perspectives on semiconductor QDs based ECL reagents are finally discussed as well.         

    Key words:electrogenerated chemiluminescence; luminophore; nanoparticle; semiconductor quantum dots

    引用本文張連梅,王宇紅,趙英杰,. 基于半導體量子點的電致化學發光試劑的研究進展[J]. 化學試劑,2022,442:169-177.

     

    基于超臨界萃取技術的泰國青檸果皮精油成分解析及其抗腫瘤活性研究

    鄭瑩1,2,3,李天嬌1,2,3,包永睿1,2,3,王帥1,2,3,楊欣欣1,2,3,趙國斌4,孟憲生*1,2,3

    1. 遼寧中醫藥大學 藥學院,遼寧 大連 116600;2. 遼寧省中藥多維分析專業技術創新中心,遼寧 大連116600;3. 遼寧省現代中藥研究工程實驗室,遼寧 大連 116600;4. 大連卓爾超臨界科技發展有限公司,遼寧 大連 116600

     

    摘要主要研究泰國青檸果皮精油成分組成及其抗腫瘤活性。采用超臨界二氧化碳萃取技術提取青檸果皮精油,超高效液相-飛行時間質譜聯用儀(UPLC-QTOF-MS氣相色譜-質譜聯用儀(GC-MS)進行成分分析,經與數據庫及參考文獻比對,鑒定化學成分;采用CCK-8測定青檸果皮精油抗肝癌細胞株HepG2和結直腸癌細胞株SW620的體外抗腫瘤活性。經UPLC-QTOF-MS指出泰國青檸果皮精油香豆素類14個、黃酮類12個、萜類6個、鞣質類1個、脂肪酸類1個;經GC-MS指出揮發性成分58個,包括醇類34個、烯烴類12個、酯類5個、醛類2個、芳香烴類2個、醚類2個和酮類1。細胞實驗證明泰國青檸果皮精油對HepG2SW620細胞株具有不同程度的抑制作用,IC50分別為0.53mg/mL0.77mg/mL,表明其具有較好的抗腫瘤活性。泰國青檸果皮精油抗腫瘤應用開發提供數據支撐。

    關鍵詞:泰國青檸果皮精油;超臨界流體萃??;抗腫瘤;UPLC-QTOF-MS;GC-MS

    中圖分類號:R9      文獻標識碼:A       文章編號0258-32832022--

     

    Component Analysis and Antitumor Activity of Oil fromKaffir Lime PeelBased on Supercritical Fluid Extraction ZHENG Ying1,2,3, LI Tian-jiao1,2,3, BAO Yong-rui1,2,3, WANGShuai1,2,3, YANG Xin-xin1,2,3, ZHAO Guo-bin4, MENG Xian-sheng*1,2,3(1. College of Pharmacy, Liaoning University of Traditional Chinese Medicine, Dalian 116600, China; 2. Liaoning Multi-dimensional Analysis of Traditional Chinese Medicine Technical Innovation Center, Dalian 116600, China; 3. Liaoning Province Modern Traditional Chinese Medicine Research and Engineering Laboratory, Dalian 116600, China; 4. Dalian Zhuoer supercritical technology development Co., Ltd, Dalian 116600), Huaxue Shiji, 2022, 44(2),

    Abstract: To study the composition and antitumor activity of oil from KaffirLime peel, oil from KaffirLime peel was extracted by supercritical carbon dioxide extraction technology. The components were analyzed by UPLC-QTOF-MS and GC-MS. These components were estimated by comparing with database and references. The antitumor activity of oil from KaffirLime peel against hepatocellular carcinoma cell line HepG2 and colorectal cancer cell line SW620 in vitro was investigated by CCK-8 assay. The results showed that by using UPLC-QTOF-MS, 14 coumarins, 12 flavonoids, 6 terpenoids, 1 tannin and 1 fatty acid were identified in the oil from KaffirLime peel. A total of 58 volatile compounds were identified by GC-MS, including 34 alcohols, 12 alkenes, 5 esters, 2 aldehydes, 2 aromatic hydrocarbons, 2 ethers and 1 ketone. Cell experiments showed that the oil from KaffirLime peel had different degree of inhibitory effects on HepG2 and SW620 cell lines, with IC50 of 0.53 and 0.77mg/mL, respectively, indicating that it had good antitumor activity. This paper provides the data support for the development of antitumor application of oil from KaffirLime peel.

    Key words: Oil from KaffirLime peel; Supercriticalfluid extraction;Antitumor;UPLC-QTOF-MS;GC-MS

    引用本文:鄭瑩,李天嬌,包永睿,. 基于超臨界萃取技術的泰國青檸果皮精油成分解析及其抗腫瘤活性研究[J]. 化學試劑, 2022,44(2):178-185。

     

     

    齊墩果酸-川芎嗪衍生物的合成及抗腫瘤活性研究

    王璇,姜曉曄,黎七雄*

    (武漢城市學院 醫學部,湖北 武漢  430083

     

    摘要: 以川芎嗪為原料,經過氧化、Boekelheide重排、水解、Ing-Manske等反應制得了兩個川芎嗪衍生物2-羥甲基-3,5,6-三甲基吡嗪和2-甲胺基-3,5,6-三甲基吡嗪,利用藥物拼合原理將其與齊墩果酸及其衍生物通過酯化或酰胺反應合成了8個新型齊墩果酸-川芎嗪衍生物,其結構通過1HNMRMS。初步的生物活性結果表明,所合成的目標化合物PC-3、MCF-7、HepG2HeLa 4種腫瘤細胞均展現出了良好的抑制活性,半數抑制濃度 (IC50)值均在20 mmol/L以內,其抗腫瘤活性明顯的強于先導化合物齊墩果酸與川芎嗪。構效關系研究表明,齊墩果酸與川芎嗪的拼接方式對活性影響不大,而齊墩果酸A環的修飾方式對活性影響較大,其中在齊墩果酸A環具有1--3-氧代官能團的化合物MCF-7展現出了最強的抑制活性,其IC50分別為3.4、2.2 mmol/L。此外,這些齊墩果酸-川芎嗪衍生物對正常MCF-10ALO2細胞沒有毒性。

    關鍵詞: 齊墩果酸;川芎嗪;拼合原理;抗腫瘤活性

    分類號R914;    文獻標記碼A     文章編號0258-32832022--

     

    Synthesis and Anti-tumor Activity Evaluation of Oleanolic acid-Ligustrazine Derivatives WANG Xuan, JIANG Xiao-ye, LI Qi-xiong* (School of Medicine, Wuhan City College, Hubei, Wuhan  430083, China), Huaxue Shiji, 2022, 44(2),

    Abstract: Initially, 2-hydroxymethyl-3,5,6-trimethylpyrazine (3) and 2-aminemethyl-3,5,6- trimethylpyrazine (6) were synthesized with ligustrazine as starting materials by oxidation reaction, Boekelheide rearrangement reaction, hydrolysis reaction, and Ing-Manske reaction. After that, eight noveloleanolic acid-ligustrazine derivatives were obtained by esterification reaction or amidation reaction of intermediate 3 or 6 with oleanolic acid or its derivatives. Their chemical structures were confirmed by 1HNMR and Mass spectra. The preliminary biological results indicated that these derivatives showed potent inhibitory activities against PC-3, MCF-7, HepG2 and HeLa cells, and their half maximal inhibitory concentration (IC50) values were less than 20 mM, which were better than that of the lead compound oleanolic acid and ligustrazine. The structure-activity relationship showed that the coupling method of oleanolic acid with ligustrazine had little effect on the antiproliferative activity, while the modification of A ring of oleanolic acid unit had obvious effect on the activity. Among them, the derivatives 17~18 with 1-en-3-oxo group in A ring of oleanolic acid unit exhibited the greatest potency against MCF-7 with the IC50 values were 3.4 and 2.2 mM, respectively. Moreover, all derivatives were nontoxic to both health MCF-10A and LO2 cells.

    Key words: oleanolic acid; ligustrazine; combination; anti-tumor activity

    引用本文王璇, 姜曉曄,黎七雄.齊墩果酸-川芎嗪衍生物的合成及抗腫瘤活性研究[J].化學試劑,2022,442):186-194.

     

    白術-白芍活性成分治療腸易激綜合征的網絡藥理學研究

    丁凌1,孫九許1,侯思瀚1,烏恩奇2,令亞琴2,裴凌鵬*1,2

    1. 中央民族大學 藥學院,北京 100081;2. 教育部 民族醫藥重點實驗室,北京 100081

     

    摘要:基于網絡藥理學的方法預測白術-白芍中活性成分治療腸易激綜合征的作用靶點、信號通路、分子機制。檢索TCMSP數據庫查找白術、白芍活性成分及其作用靶點。檢索OMIM、GenecardDrugbank數據庫富集疾病靶點并篩查交集靶點。采用String數據庫與Cytoscape軟件進行蛋白相互作用分析、靶點網絡構建。通過Metascape數據庫進行通路富集分析與功能注釋。最終篩選出活性成分20個,作用靶點73個,交集靶點61個?;钚猿煞职?/span>3β-乙酰氧基蒼術酮、β-谷甾醇、山萘酚等。作用到的核心靶點包括白細胞介素-6 (IL-6)、蛋白激酶1 (AKT1)、腫瘤壞死因子 (TNF)等。通路富集分析得到121條信號通路,包括腫瘤壞死因子信號通路、白介素-17信號通路、Toll樣受體信號通路等,以晚期糖基化終產物及其胞膜受體信號通路最為顯著。功能注釋分析得到生物進程條目261個,以調節蛋白同源二聚體的活性最為顯著;分子功能條目62個,以對脂多糖、細菌來源分子等成分的反應為主。白術-白芍發揮治療腸易激綜合征的作用是多成分、多靶點、多途徑作用的結果。

    關鍵詞:網絡藥理學;活性成分;腸易激綜合征;白術;白芍;潛在靶點;信號通路

    中圖分類號R282.71        文獻標碼:A        文章編號:0258-32832022- -

     

    Study on Effective Substances of Atractylodes macrocephala Koidz - Paeonia lactiflora Pall in Treatment of Irritable Bowel Syndrome Based on Network Pharmacology DING Ling1, SUN Jiu-xu1, HOU Si-han1, WU En-qi2, LING Ya-qin2, PEI Ling-peng*1,2(1.School of Pharmacy, Minzu University of China, Beijing, 100081, China; 2. Key Laboratory of Ethnomedicine, Ministry of Education, Beijing, 100081, China), Huaxue shiji, 2022, 44(2),

    AbstractBased on network pharmacology, the potential targets, signaling pathways and molecular mechanism of active components among Atractylodes macrocephala Koidz and Paeonia lactiflora Pall in the treatment of irritable bowel syndrome are predicted. The active components and potential targets of Atractylodes macrocephala Koidz and Paeonia lactiflora Pall were retrieved by the TCMSP database, while the potential targets of irritable bowel syndrome were screened by OMIM, GeneCards and Drugbank databases. By finding common targets among the above potential targets, a protein-protein interaction network has been analyzed and constructed through String database and Cytoscape software. KEGG pathway enrichment analysis and GO biological function module analysis of key targets were performed by Metascape database. Totally 20 active components of Atractylodes macrocephala Koidz and Paeonia lactiflora Pall were screened out, including 3β-acetoxyatractylone, β-sitosterol, kaempferol, etc. 73 relative targets were found from the components above, and 61 targets of the massociated with diseases. The core targets mainly included IL-6, AKT1, TNF, etc. KEGG analysis revealed 121 signaling pathways like TNF, IL-17 and Toll-like Receptor with the AGE-RAGE signaling pathway being the most significant. GO analysis revealed 261 biological process entries, among which protein homodimerization activity were the most significant one. Moreover, 62 molecular function entries were being revealed,the response of which to lipopolysaccharide and molecule of bacterial origin were the most important. Atractylodes macrocephala Koidz and Paeonia lactiflora Pall performs the role of multiple-components, multiple-targets, and multiple-pathways in treatment of irritable bowel syndrome.

    Key words: network pharmacology; active components; irritable bowel syndrome; Atractylodes macrocephala Koidz; Paeonia lactiflora Pall; potential targets; signaling pathway

    引用本文丁凌,孫九許,侯思瀚,. 白術-白芍活性成分治療腸易激綜合征的網絡藥理學研究[J]. 化學試劑,2022,44(2):195-202。

     

     

    基于1,8-萘酰亞胺的甲醛熒光探針研究進展

    曹碧霞1,2,劉*1,2,高玉清1,劉婷1,岳勝利1

    (1. 甘肅省化工研究院有限責任公司,甘肅 蘭州  730020;2. 甘肅省精細化工重點實驗室,甘肅 蘭州  730020)

     

    摘要:甲醛廣泛存在于工業生產和日常生活中,是常見的環境污染物和人體致癌物。1,8-萘酰亞胺是重要的雙光子熒光基團,具有良好的光穩定性、大的stocks位移以及高的熒光量子產率。近年來,大量基于1,8-萘酰亞胺基團的甲醛熒光探針被開發出來,并在環境監測及生命科學等領域有了較為初步的應用。對甲醛與識別基團的反應類型分類,綜述了近年來具有代表性的基于1,8-萘酰亞胺基團的甲醛熒光探針的最新研究進展,并展望了其未來設計與發展趨勢。

    關鍵詞:甲醛;1,8-萘酰亞胺;熒光探針;設計;進展

    中圖分類號:O65           文獻標記碼A     文章編號0258-32832022--

     

    Research Progress of Formaldehyde Fluorescent Probes Based on 1,8-naphthimide CAO Bi-xia1,2, LIU Rong*1,2, GAO Yu-qing1, LIU Ting1, YUE Sheng-li1 (1. Gansu Research Institute of Chemical Industry Co., Ltd., Lanzhou, 730020, China; 2. Gansu Key Laboratory of Fine Chemicals, Lanzhou, 730020, China), Huaxue Shiji, 2022, 44(2),

    Abstract: Formaldehyde widely exists in industrial production and daily life, which is a common environmental pollutant and human carcinogens. 1,8-naphthimide is an important two-photon fluorescence group, which has good photostability, large stocks shift and high fluorescence quantum yield. In recent years, a large number of formaldehyde fluorescent probes based on 1,8-naphthimide groups have been developed, and they had been preliminary applied in the fields of environmental monitoring and life sciences. This article categorizes the reaction types of formaldehyde and recognition groups, summarizes the latest research progress of representative formaldehyde fluorescent probes based on 1,8-naphthimide in recent years, and gives the prospect in future design and development trends.

    Key words: formaldehyde; 1,8-naphthimid; fluorescent probes; design; progress

    引用本文:曹碧霞,劉 榮,高玉清,等.基于1,8-萘酰亞胺的甲醛熒光探針研究進展[J].化學試劑,2022,442:203-211.

     

     

    基于碳納米點熒光試紙可視化探針的構建及應用

    黃誠*1,張帥帥1,權一鳴1,任科旭1,田燕琳1,朱森強2,劉睿2

    (1. 東南大學成賢學院 制藥與化學工程學院,江蘇 南京  210088;2. 南京工業大學 化學與分子工程學院,江蘇 南京  211816

     

    摘要:以吩噻嗪為原料,經硝化反應合成出3,7-二硝基吩噻嗪,并以此為前驅體,制備出兩種N、S摻雜的碳納米點材料,通過多種手段對所合成材料結構和組成進行表征。將碳納米點應用于Cu2+的快速定性/定量可視化檢測,并基于碳納米點熒光試紙結合智能手機的顏色分析識別,構建Cu2+可視化檢測傳感器,展現出高效、準確、靈敏和便捷的優勢。在05 μmol/L范圍內的碳納米點熒光差值和Cu2+濃度的相關系數R2 = 0.9976,Cu2+檢出限可達0.26 μmol/L;015 μmol/L范圍內,試紙熒光顏色的B/R值與Cu2+濃度呈現較好的線性關系,相關系數R2 = 0.9213,Cu2+檢出限可達1.28 μmol/L。熒光試紙的開發和應用為功能化碳納米點材料提供了有益思路,有望應用于現場和實時檢測中。

    關鍵詞:硝化反應;碳納米點;熒光試紙;智能手機;可視化傳感

    中圖分類號:O69       文獻標識碼:A       文章編號:0258-3283(2022)--

     

    Construction and Application of Visual Sensor Based on Carbon Nanodots Fluorescent Test Paper HUANG Cheng*1, ZHANG Shuai-shuai1, QUAN Yi-ming1, REN Ke-xu1, TIAN Yan-lin1, ZHU Sen-qiang2, LIU Rui2 (1. Department of Chemical and Pharmaceutical Engineering, Southeast University Chengxian College, Nanjing 210088, China;2. College of Chemistry and Molecular Engineering, Nanjing Tech University, Nanjing 211816, China), Huaxue Shiji,2022, 44(2),

    Abstract: Aromatic nitro compounds were synthesized through nitration reaction by using phenothiazine, and used to preparetwo N, S-doped carbon nanodots (CNDs). These synthesized materials were characterized by various methods. The obtained CNDs were applied to the rapid qualitative, quantitative visualization detection of Cu2+. Based on the fluorescent test paper of CNDs and the color analysis and recognition of smart phones, a visual detection sensor for Cu2+ is constructed, which is effective, accurate, sensitive and convenient. Thefluorescence difference of CNDs and Cu2+ concentration in the range of 05 μmol/L show a good linearity, the correlation coefficient R2 = 0.9976, and the detection limit can reach 0.26μmol/L. In the range of 015 μmol/L, the B/R value of fluorescent test paper shows a good linear relationship with Cu2+ concentration, the correlation coefficientR2 = 0.9213, and the detection limit of Cu2+ can reach 1.28 μmol/L. The development and application of the test paper provides a useful idea for functionalized CNDs materials, and is expected to be applied to field and real-time detection.

    Keywords: nitration reaction; carbon nanodots; fluorescent test paper; smart phone; visual sensing

    引用本文黃誠,張帥帥,權一鳴,等. 基于碳納米點熒光試紙可視化探針的構建及應用[J]. 化學試劑,2022,44(2):212-218。

     

     

    基于萘酚席夫堿結構的熒光增強型鋁離子探針

    劉玉村*,于曉凡,趙妍,吳淼,王媛,趙際涵

    (吉林師范大學 化學學院,吉林 四平  136000)

     

    摘要:金屬離子Al3+在生命系統中起著非常重要的作用并影響著人類的健康,熒光分子探針由于方法簡單、選擇性和靈敏度高、現場實時監測、檢出限低等優點吸引了更多的研究關注。通過一步縮合反應制備了基于萘酚席夫堿結構的熒光分子探針,該分子探針DMSO/H2O溶液中對Al3+具有較好的選擇性。加入Al3+后分子探針溶液的熒光強度明顯增強,且溶液發射出明顯的藍綠色熒光。同時,分子探針對Al3+表現出較好的靈敏度,其檢測限為1.58×10-8 mol/L。分子探針與Al3+2 1結合模式進行配位,pH實用范圍為6 ~ 9,且具有可逆性。此外,分子探針可對實際飲用水中的Al3+進行定量檢測。

    關鍵詞:萘酚;席夫堿;熒光增強;鋁離子;探針

    中圖分類號:O655.9       文獻標識碼:A       文章編號:0258-32832022

     

    A Fluorescence Enhancement Al3+ Probe Based on Naphthol Schiff Structure Liu Yu-cun*, YU Xiao-fan, Zhao Yan, Wu Miao, Wang Yuan, ZhaO Ji-han (College of Chemistry, Jilin Normal University, Siping 136000, China), HuaxueShiji, 2022

    Abstract: The metal ion Al3+ plays very important roles in living system and affects human health. Fluorescence probes with simple method, high selectivity and sensitivity, real-time monitoring and low detection limit have aroused more attention. A fluorescent probe based on naphthol Schiff base structure was prepared by one-step condensation reaction. The probe showed good selective for the detection of Al3+ in DMSO/H2O solution. Upon the addition of Al3+, the fluorescence intensity of solution was significantly enhanced, and the solution emitted obvious blue-green fluorescence. In addition, the probe also exhibited good sensitivity to Al3+ with a detection limit of 1.58×10-8 mol/L. The probe was found to bind with Al3+in a 2:1 (probe: metal) stoichiometric fashion. The probe had good recognition performances for Al3+ in the range of pH = 6 ~ 9, and the sensing process was chemically reversible by adding EDTA. Furthermore, the probe could be successfully practiced for the quantitative analysis of Al3+ in actual water samples.

    Key words: naphthol; Schiff base; fluorescence enhancement; Al3+; probe

    引用本文:劉玉村,于曉凡,趙妍,等.基于萘酚席夫堿結構的熒光增強型鋁離子探針[J]. 化學試劑,2022, 44(2):219-223.

     

     

    新型咔唑衍生物的合成及發光性能研究

    曹建華*1,李敏2,趙雷1,韓洪波1,田會強1,鄧師勇1

    1. 北京八億時空液晶科技股份有限公司,北京  102500;2. 中國政法大學 商學院 工商管理系,北京  100088

     

    摘要基于螺二芴的大位阻結構和咔唑的高三線態能級,設計了一種在咔唑的3、45、6位并入兩個高位阻的螺二芴結構,以4,4’-二甲基聯苯為起始原料,經過硝化反應、Bucherer反應、偶聯反應、鹵化、Suzuki偶聯反應和關環等反應成功制備了咔唑衍生物CzSF2,產物結構經過1H NMR、13C NMR、MS確證。其在二氯甲烷溶液中的最強發射峰位于384 nm,磷光發射峰位于450 nm,CzSF2ES1ET1分別為3.4 eV2.88 eV。分別以CzSF2mCBP3,3’-Di(9H-carbazol-9-yl)biphenyl為磷光主體材料,分別摻雜3%、6%10%GD030((2-氘甲基-8-2-吡啶基苯并呋喃[2,3-b]吡啶2-苯基吡啶III))制備了綠色磷光電致發光器件PhOLEDs,在較低3%摻雜濃度下,實現了較高的電流效率、功率效率和外量子效率,分別為98.5 cd/A、83.0 lm/W25.2%,與mCBP作為主體材料相比,驅動電壓低約11%、發光效率高約4%。研究結果表明:利用高度扭曲的螺二芴共軛結構和位阻優勢以及高π-π共軛的咔唑設計合成的材料CzSF2具有高的熱穩定性,高的三線態能級,非常適用于有機電致發光二極管的發光層,用于磷光主體材料,本征光電性能良好,設計思路對實現低濃度銥配合物的摻雜具有借鑒意義。

    關鍵詞4,4’-二甲基聯苯;螺二芴;咔唑;有機電致發光材料;磷光主體材料 

    中圖分類號:O626.2    文獻標識碼:A       文章編號:0258-32832022--

     

    Synthesis and Luminescent Properties of New Carbazole Derivatives CAO Jian-hua*1, LI Min2, ZHAO Lei1, HAN Hong-bo1, TIAN Hui-qiang1, DENG Shi-yong1 (1. Beijing Bayi Space LCD Technology Co., Ltd., Beijing 102500, China; 2. Department of Business Administration, Law Business School, China University of Political Science, Beijing 100088, China), Huaxue Shiji, 2022, 44(2),

    AbstractBased on the large steric hindrance of spirobifluorene and the high triplet energy level of carbazole, we designed a carbazole derivative, structure of which has two spirobifluorenes at 3,4 and 5,6 positions of carbazole. By using 4,4'-dimethylbiphenyl as starting material, the double 9,9'-spirobifluorenes and one carbazole derivative CzSF2 was synthesized via sequential reactions of nitration, Bucherer reaction, coupling, halogenations, Suzuki-Miyaura coupling, cyclization reaction and other reactions. All compounds were identified by 1H NMR, 13C NMR and MS spectra. The optical and electronic properties have been investigated by molecular simulation and calculation. The emission spectrum of CzSF2 showed a maximum peak at 384 nm and a shoulder peak at 403 nm, and the phosphorescence emission peak located at 450 nm at low temperature, therefore, the ES1 and ET1 were calculated to be 3.4 eV and 2.88 eV, respectively. CzSF2 and mCBP are used asthe phosphorescent host materials, and the green phosphorescent organic light-emitting diodes devices (PhOLEDs) were fabricated by doping with ω3%, ω6% and ω10% of iridium complex GD030 (2-(methyl-d3)-8-(pyridin-2-yl)benzofuro[2,3-b] pyridine)bis[2-phenylpyridinato-C2,N]Ir(III)), respectively. The highest current efficiency, power efficiency and external quantum efficiency were achieved in low (3%) doping concentrations, which were 98.5 cd/A, 83.0 lm/w and 25.2%, respectively, under current density of 0~100 mA/cm2.Compared with mCBP as the host material, the driving voltage is 11% lower and the luminous efficiency is about 4% higher. These results indicate that the material of CzSF2,designed by taking advantages of the highly twisted spirobifluorene conjugated structure, steric hindrance and the high π-π conjugated carbazole, has high thermal stability and high triplet energy level, which is suitable for organic electroluminescence. The light-emitting layer of the OLEDs is used as the phosphorescent host material that has good intrinsic photoelectric performance. The design ideas of host material have reference significance to realize the dopant with lower concentrations of iridium complex.

    Key words: 4,4'-dimethylbiphenyl; spirobifluorene; carbazole; organic electroluminescent materials; phosphorescent host material

    引用本文:曹建華,李敏,趙雷,等. 新型咔唑衍生物的合成及發光性能研究[J]. 化學試劑, 2022, 44(2):224-232。

     

     

    Cu-N/C單原子催化劑用于芳基硼酸羥基化反應

    李曉怡1,朝飛1,麥悅賢1,梁廣鋒1,郎睿*1,吳傳德*2

    1.廣東工業大學 輕工化工學院,廣東 廣州  510006;2.浙江大學 化學學院,浙江 杭州  310027

     

    摘要:單原子催化劑中所有金屬原子都能作為活性位點,故表現出極高的原子利用率和優異的催化性能。以銅-乙二胺四乙酸配合物作為前驅體,高比表面的活性炭作為載體,通過簡單的吸附浸漬-高溫焙燒法制備了一系列Cu-N/C催化劑。結果發現,當銅負載量為0.2wt%時,銅以單原子的狀態分散在載體上,得到0.2wt%Cu-N/C(1:1)單原子催化劑。該催化劑在芳基硼酸羥基化制苯酚的反應中具有優異的活性,可以直接用氧氣作為氧化劑,反應效率達到3250 mmol產物/gCu,高于銅納米顆粒催化劑6倍。此外,該單原子催化劑穩定性較好,并且該反應對各種帶有吸電子或給電子基團的芳基硼酸都具有良好的底物適用性。

    關鍵詞:銅;單原子催化;苯硼酸;羥基化反應;炭載體

    中圖分類號:O643        文獻標識A     文章編號0258-32832022--

     

    Ipso-hydroxylation of Aryl boronic Acids Catalyzed by Cu-N/C Single-Atom Catalyst LI Xiao-yi1, CHAO Fei1, MAI Yue-xian1, LIANG Guang-feng1, LANG Rui*1, WU Chuan-de*2 (1.School of Chemical Engineering and Light Industry, Guangdong University of Technology, Guangzhou 510006, China; 2.Department of Chemistry, Zhejiang University, Hangzhou 310027, China), Huaxue Shiji, 2022, 44(2),

    Abstract: Single-atom catalysts can improve the catalytic performance by maximizing the atomic efficiency of active metal species, thus exhibiting high catalytic performance. In this paper, a series of Cu-N/C catalysts were prepared by impregnating active carbon material with Cu-EDTA complex precursor and the subsequent calcination. The composition and morphology of the catalyst were characterized by the combination of XRD, AC-STEM, and BET techniques. The synthesized 0.2wt%Cu-N/C(1:1) single-atom catalyst carries out the ipso-hydroxylation of phenylboronic acid to produce phenol under O2 atmosphere with a catalytic efficiency of 3250 mmolproduct/gCu, which was6 times higher than that of Cu nanoparticle catalyst. In addition, this single-atom catalyst shows good stability and wide functional-group tolerance, because various arylboronic acids with electron withdrawing/donating groups can be transformed to the corresponding phenolic compounds under mild conditions.

    Key words:copper; single-atomcatalysis; phenylboronic acid; ipso-hydroxylation; carbon support

    引用本文李曉怡,朝飛,麥悅賢,等. Cu-N/C單原子催化劑用于芳基硼酸羥基化反應[J]. 化學試劑,2022,44(2):233-238.

     

     

    星點設計-效應面法優化羧甲基殼聚糖包覆納米粒處方工藝

    黃欣瑜,何李浩,姜佳妙,夏曉靜*

    (浙江醫藥高等??茖W校藥學院,浙江寧波 315100

     

    摘要:為獲得包封率高且穩定的載齊墩果酸的羧甲基殼聚糖包覆納米制劑。采用星點設計-效應面法進行優化,以粒徑、電位、包封率為評價指標,非線性數學模型擬合,并對優選出的條件制成的納米粒進行粒徑、電位等評價,HPLC法進行載藥量測定及體外釋放評價。優化后條件為醇水比為0.105,單硬脂酸甘油酯與硬脂酸比為1.656,羧甲基殼聚糖與硬脂酸比為1.458,制備所得納米粒包封率93.4納米粒包封,載藥量為9.1量為米粒包,粒徑362.3米粒包封nm,電位-44.8米粒包封mV,體外釋放也說明納米粒能維持48h以上載藥穩定。該法優化后所得測量值與預測值偏差較小,相關性好,為齊墩果酸殼聚糖包覆納米粒的處方設計提供了可靠的依據。

    關鍵詞星點設計-效應面法;羧甲基殼聚糖;納米粒;齊墩果酸

    中圖分類號:R944;R975文獻標識碼:A文章編號:0258-32832022

     

    Optimiazation of Formulation and Preparation Technology of Carboxymethyl Chitosan-Coated Nanoparticle by Central Composite Design and Response Surface Methodology HUANG Xin-yu, HE Li-hao, JIANG Jia-miao, XIA Xiao-jing* (Department of Pharmaceutics, Zhejiang Pharmaceutical College, Ningbo315100, China), Huaxue Shiji, 2022, 44(2),

    Abstract: To obtain stable carboxymethyl chitosan-coated nanoparticles loading oleanolic acid with high encapsulation efficiency, the central composite design response surface method was used to optimize the formulation and preparation of the nanoparticles which take particle size, potential, and encapsulation efficiency as evaluation indexes. And also a nonlinear mathematical model was fitted. The particle size and potential of the optimized formulation were evaluated, and the drug loading andthe in-vitro release were determined by HPLC. The optimized conditions were as follows: the alcohol-water ratio was 0.105,the proportion of glyceryl monostearate(GM) to stearic acid(SA) was 1.656, and that carboxymethyl chitosan(C-Cs) to SA was 1.458. Encapsulation efficiency of the optimized nanoparticles was 93.4 ± 2.8%, drug loading was 9.1 ± 1.6%, particle size was 362.3 ± 7.2nm, and zetapotential was - 44.8 ± 0.9mv. The in vitro release showed that the nanoparticles were stable enough for more than 48h. This optimized method provides a reliable basis for the formulation design of oleanolic acid chitosan-coated solid lipid nanoparticles.

    Key words: central composite design and response surface methodology; carboxymethyl chitosan; nanoparticle; oleanolic acid

    引用本文:黃欣瑜,何李浩,姜佳妙,等. 星點設計-效應面法優化羧甲基殼聚糖包覆納米粒處方工藝[J]. 化學試劑, 2022, 44(2): 239-244.

     

     

    光誘導錳羰基化合物釋放一氧化碳研究

    張俊蝶,王雪梅,潘瀅瀅,吳曉君,李愛云,姜秀娟*

    (嘉興學院 生物與化學工程學院,浙江 嘉興  314001)

     

    摘要通過合成可見光誘導的一氧化碳釋放分子,實現可見光作用下的一氧化碳釋放。通過Mn(CO)5Br和鄰菲羅啉衍生物反應合成得到了一種光敏感的錳羰基化合物[Mn(CO)3(L)Br] ,并進一步通過紅外光譜和紫外光譜技術研究了該化合物在不同可見光作用下的一氧化碳(CO)釋放性能。結果表明,目標化合物在可見光作用下即可分解釋放CO,可以作為潛在的光誘導一氧化碳釋放分子。進一步研究其CO釋放動力學表明該過程符合準一級反應模型,而且CO放速率可通過選用不同光源進行調控。因此,通過得到一種速率方便調控的可見光誘導的一氧化碳釋放劑,預期該化合物在醫藥領域具有潛在的應用前景。

    關鍵詞一氧化碳釋放劑;錳羰基化合物;光誘導;鄰菲羅琳衍生物

    中圖分類號:O614.8    文獻標識碼:A       文章編號:0258-3283(2022)--

     

    The Study of Photo Initiation Carbon Monoxide releasing from Manganese Carbonyl Complex ZHANG Jun-die, WANG Xue-mei, PAN Ying-ying, Wu Xiao-jun, LI Ai-yun, JIANG Xiu-Juan* (, College of Biological and Chemical Sciences and Engineering, Jiaxing University, Jiaxing 314001, China), Huaxue Shiji, 2022, 44(2),

    AbstractPhotoinduced carbon monoxide releasing agent has attracted extensive attention of scientists because of its easy controllability. In this paper, we have synthesized visible light induced carbon monoxide releasing molecule to realize carbon monoxide releasing under visible light. Alight-sensitive manganese carbonyl compound [Mn(CO)3(L)Br] (1) was synthesized by the reaction of Mn(CO)5Br and phenanthroline derivative. Its carbon monoxide releasing ability under different visible light were studied by infrared and ultraviolet spectroscopy. The results showed that compound 1 could decompose and release CO under visible light, and be used as a potential photoinduced carbon monoxide releasing molecule (photoCORMs). Further study of the CO release kinetics revealedthat the process conforms to the quasi-first-order reaction model, and the CO release rate can be controlled by selecting different light sources. This work provides a visible light induced carbon monoxide releasing agentwith easy rate regulation, which is expected to have a potential application in the medical field.

    Key wordsCO-releasing moleculeCORMs; manganese carbonyl complex; photo initiation; phenanthroline derivatives 

    引用本文: 張俊蝶,王雪梅,潘瀅瀅,等. 光誘導錳羰基化合物釋放一氧化碳研究[J].化學試劑,2022,442245-249.

     

     

    金屬酞菁/卟啉分子電催化CO2還原的研究進展

    曹茂啟,吳大旺,李曉鳳,向丁玎,羅駿,李云萍,代虹鏡*

    (黔南民族師范學院 化學化工學院,貴州 都勻 558000

     

    摘要:大氣中日益增加的CO2濃度導致了氣候變化等環境問題。將CO2催化轉化為有價值的化學品具有重要意義。利用太陽能、風能等可再生能源產生的電能,通過電化學方法將CO2還原轉化為有價值的碳基化合物是最具有應用前景的方式。分子催化劑具有明確的結構和清晰的活性位點,可實現基于機理的性能優化。綜述了近年來金屬酞菁/卟啉分子在電催化CO2還原為CO的實驗和理論方面的最新研究進展。首先,介紹了金屬酞菁/卟啉分子電催化CO2還原為CO的詳細機理。然后,重點介紹了如何通過分子分散和配體修飾提升金屬酞菁/卟啉分子電催化CO2還原為CO的活性和選擇性。最后,討論了金屬酞菁/卟啉分子電催化CO2還原存在的挑戰及其可能的解決方案。

    關鍵詞:金屬酞菁/卟啉基分子;碳納米材料;電催化CO2還原;反應機理;活性和選擇性

    中圖分類號:O643.3        文獻標識碼:A      文章編號:0258-32832022--

     

    Research Progress of Electrocatalytic Reduction of CO2 by Metal Phthalocyanine/Porphyrin Molecules CAO Mao-qi, WU Da-wang, LI Xiao-feng, XIANG Ding-ding, LUO Jun, Li Yun-ping, DAI Hong-jing* (School of Chemistry and Chemical Engineering, Qiannan Normal University for Nationalities, Duyun 558000, China), Huaxue Shiji, 2022, 44(2), 

    Abstract: The increasing concentration of CO2 in the atmosphere contributes to environmental problems such as climate change. The catalytic conversion of CO2 into valuable chemicals is of great significance. It is the most promising way to use the electric energy provided by solar energy, wind energy and other renewable energy to reduceCO2 into valuable carbon-based compounds by electrochemical method. The molecular catalyst has distinct structures and clear active sites, which is conducive to the optimization of performance based on the mechanism. The latest experimental and theoretical research in the electrocatalytic reduction of CO2 to CO by metal phthalocyanine/porphyrin molecules in recent years was reviewed. Firstly, we introduced the detailed mechanism of electrocatalytic of CO2 to CO. And then, we focused on how to improve the activity and selectivity of electrocatalytic of metal phthalocyanine/porphyrin molecules for reducingCO2 to CO through molecular dispersion and ligand modification. Finally, we discussed the challenges and possible solutions of metal phthalocyanine/porphyrin molecular in the process of electrocatalytic CO2 reduction.

    Key words: metal phthalocyanine/porphyrin molecules; carbon nanomaterials; electrocatalytic reduction of carbon dioxide; reaction mechanism; activity and selectivity

    引用本文:曹茂啟,吳大旺,李曉鳳,等. 金屬酞菁/卟啉分子電催化CO2還原的研究進展[J]. 化學試劑, 2022, 44(2)250-258。

     

     

    改性花生殼吸附亞甲基藍動力學與機理研究

    呂東燦,王志敏,姜廣策,王佳雯,李演鑫,朱乾臣,李鑫*

    (河南農業大學 理學院,河南 鄭州  450002

     

    摘要:吸附法是去除水中有機污染物的一種重要方式。以農業廢棄物花生殼為原料,通過稀酸改性制備對亞甲基藍吸附性能良好的生物質基吸附材料。FTIR分析表明改性花生殼表面含有羥基、羧基等有利于吸附的官能團,SEM和孔結構分析結果顯示稀硫酸改性花生殼表面形成大量孔結構。亞甲基藍濃度為100 mg/L時,改性花生殼的去除效率為91.5%。亞甲基藍吸附過程符合準二級動力學,熱力學數據符合LangmuirRedlich-Peterson模型,表明改性花生殼對亞甲基藍是化學吸附為主的單分子層吸附過程,氫鍵、范德華力和電子作用是吸附的主要機理。Langmuir擬合可知稀硫酸改性花生殼對亞甲基藍的最大吸附量為174.9 mg/g。這種價廉、高效的生物質基吸附材料為低成本、環境友好地利用廢棄生物質資源提供了理論依據。

    關鍵詞:花生殼;硫酸預處理;動力學;亞甲基藍;機理

    中圖分類號:S52;TQ352         文獻標碼:A         文章編號:0258-32832022--

     

    Adsorption Kinetics and Mechanism of Sulfuric Acid Modified Peanut Husk for Removal of Methylene Blue LV Dong-can, WANG Zhi-min, Jiang Guang-ce, WANG Jia-wen, LI Yan-xin, ZHU Qian-chen, LI Xin* (College of Science, Henan Agricultural University, Zhengzhou 450002, China), Huaxue Shiji, 2022, 44(2),

    Abstract: Adsorption is an important pathway for removal of organic pollutant from water. The present study aimed at the removal of methylene blue (MB) using peanut hull modified by sulphuric acid treatment. FTIR showed that there are plenty of hydroxyl and carboxyl groups, as well as other functional groups, conducive to adsorption. Scanning electron microscope (SEM) results showed that a rough surface with pore structure was presented on the modified peanut hull surface, which was confirmed by specific surface area analysis. The removal efficiency was 91.5% under the MB initial concentration of 100 mg/L. For H2SO4 modified sorbents tested, pseudo-second-order model was more suitable for fitting adsorption, and MB adsorption followed both Langmuir and Redlich-Peterson model. The MB removal was a monolayer adsorption process dominated by chemisorption, which was also a spontaneous and endothermic process. Adsorption mechanisms involve hydrogen bonds, electrostatic, and Van der Waals force. The maximum absorption capacity is 174.9 mg/g by Langmuir model. The results suggest that the modified agricultural waste is an environmentally friendly and low-cost bio-sorbent for effective removal of MB from aqueous solutions.

    Key words: peanut hull; sulphuric acid pretreatment; adsorption kinetics; methylene blue; mechanism

    引用本文呂東燦,王志敏,姜廣策,等. 改性花生殼吸附亞甲基藍動力學與機理研究[J]. 化學試劑,2022,44(2)259-265.

     

     

    基于高分辨質譜技術的植物源性藥食同源特色農產品中10種農藥殘留的測定和快速篩查

    謝昊臻1,胡婷婷2,王佳慧2,付瑤2,陳光宇2,李愛軍2,榮會2,張勛*2,張哲*1

    (1.  長春中醫藥大學吉林省人參科學研究院,吉林 長春 130118;2. 長春海關技術中心,吉林 長春 130062

     

    摘要:建立了人參、五味子、刺五加、人參花、靈芝和靈芝孢子粉基質中10種農藥殘留的高分辨液相質譜檢測及篩查方法,樣品中殘留的農藥采用乙腈提取,經氯化鈉及乙酸鈉鹽析分層,提取液經無水硫酸鎂、N-丙基乙二胺(PSA)石墨化炭黑(GCB)吸附劑分散固相萃取凈化,用高效液相色譜-高分辨質譜定性。在上述檢測方法條件下,所測的10種農藥的定量限為10 μg/kg,平均回收率為73.2%98.5%,線性范圍為101000 μg/LR2>0.9986)。本研究所建立的方法前處理簡單快捷,能夠快速篩查出樣品中的10種農藥并對目標物進行準確的定性分析,為藥食同源特色農產品中的農藥殘留的風險評估提供了技術支持。

    關鍵詞:藥食同源;農藥;高效液相色譜;高分辨質譜;快速篩查法

    中圖分類號:O657.63    文獻標識碼:A    文章編號:0258-32832022--

     

    Determination and Rapid Screening of 10 Pesticide Residues in Agricultural Products of Plant Origin Medicine Homologous Food by High Resolution Mass Spectrometry XIE Hao-zhen1, HU Ting-ting2, WANG Jia-hui2, FU Yao2, CHEN Guang-yu2, LI Ai-jun2, RONG Hui2, ZHANG Xun*2, ZHANG Zhe*1 (1.Jilin Ginseng Academy, ChangChun University Of Chinese Medicine, Changchun 130117; 2. Changchun Customs Technology Center, Changchun 130062, China), Huaxue Shiji, 2022, 44(2),

    Abstract: A high-resolution liquid chromatography-mass spectrometry (HPLC-MS) method was developed for the detection and screening of 10 pesticide residues in ginseng, Schisandrachinensis, acanthopanaxsenticosus, ginseng flower, Ganodermalucidum and Ganodermalucidum spore powder. The pesticide residues were extracted with acetonitrile, salted out by sodium chloride and sodium acetate, and then purified by solid phase extraction with anhydrous magnesium sulfate, PSA and GCB. The samples were identified by high performance liquid chromatography high resolution mass spectrometry. Under the above conditions, LOQ of 390 pesticides was 10 μg/kg. The average recovery was 80.5%96.6% and the linear range was 101000 μg/L (R2> 0.9986). This established method was simple and rapid. Quickly screening out samples of 10 kinds of pesticides and accurately qualitative analysis provides a technical support for the medicine edible characteristic agricultural products pesticide risk assessment.

    Key words: medicine homologous food; pesticide; high performance liquid chromatography (HPLC); high resolution mass spectrometry; rapid screening method

    引用本文謝昊臻,胡婷婷,王佳慧,等.基于高分辨質譜技術的植物源性藥食同源特色農產品中10種農藥殘留的測定和快速篩查[J]. 化學試劑, 2022, 44(2): 266-272。

     

     

    固相萃取法與GC-FPD聯用分析海水中13種有機磷

    彭詩琪1,2,3,趙嘉輝1,3,黃曉玲1,3,吳志鵬1,3,張傲1,3,陳婷2,賴華杰*1,3

    (1. 中科檢測技術服務(廣州)股份有限公司,廣東 廣州  510650;2. 中科廣化(重慶)新材料研究院有限公司,重慶  400700;3. 中國科學院廣州化學有限公司,廣東 廣州  510650

     

    摘要有機磷農藥的廣泛使用導致其不可避免地進入到環境中,不僅會影響生態環境,而且還會通過食物鏈富集進入到人體中,對人類健康造成影響。建立了固相萃取與GC-FPD聯用的方法,并成功用于海水樣品中敵敵畏等13種有機磷的分析。在中性條件下,100 mL水樣經過HLB固相萃取小柱富集后,以二氯甲烷為洗脫溶劑進行洗脫,以HP-5柱為分離色譜柱,FPD為檢測器,實現了對13種有機磷的分離及檢測。對固相萃取柱和洗脫溶劑的種類、儀器條件等進行了探究,比較了C18、HLB、PSD 3種固相萃取柱對有機磷的吸附性能以及丙酮、二氯甲烷、乙酸乙酯3種溶劑的洗脫能力,考察了海水的基質效應對有機磷分析的影響。在最優的分析條件下,13種有機磷可實現基線分離,線性良好,相關系數均大于0.995,回收率在58.3%~114%之間,所建方法適用于海水樣品中敵敵畏等13種有機磷的同時測定。

    關鍵詞:有機磷;海水;固相萃??;氣相色譜;基質效應;敵敵畏

    中文分類號:O657.7      文獻標識碼:A      文章編號:0258-32832022--

     

    Determination of 13 Kinds of Organophosphorus Pesticides in Seawater by Solid Phase Extraction Coupled with Gas Chromatography-flame Photometric DetectorPENG Shi-qi1,2,3, ZHAO Jia-hui1,3, HUANG Xiao-ling1,3, WU Zhi-peng1,3, ZHANG Ao1,3, CHEN Ting2, LAI Hua-jie*1,3 (1. CAS Testing Technical Services GuangzhouCo., Ltd., Guangzhou 510650, China; 2. New Materials Research Institute of CASCHEMChongqingCo., Ltd., Chongqing 400700, China; 3. Guangzhou Institute of Chemistry, Chinese Academy of Science, Guangzhou 510650, China), Huaxue Shiji, 2022, 44(2),

    Abstract: The widespread abuse of organophosphorus pesticides leads to the inevitable release into environment, which not only affects the ecological environment, but also causes harm to human health through the enrichment of the food chain. The method of solid phase extraction (SPE) coupled with GC-FPD was established and successfully applied for the determination of 13 kinds of organophosphorus pesticides in seawater samples such as dichlorvos, etc. Under neutral condition, 100mL water sample was enriched by HLB column, and then dichloromethane was used for elution. The separation and determination of 13 kinds of organophosphorus pesticides was completed by using HP-5 as the chromatography column and FPD as the detector. The types of solid phase extraction column, elution solvent, and instrument condition were optimized. The adsorption performance of C18, HLB and PSD solid phase extraction columns for organophosphorus pesticides and the elution capacity of acetone, dichloromethane and ethyl acetate were compared, and the matrix effect was investigated. Under the optimized conditions, the separation baseline of analytes was achieved. The linear coefficients of analytes were more than 0.995, and the recovery rates were between 58.3~114%. The established method was suitable for simultaneous determination of 13 kinds of organophosphorus pesticides.

    Key words: organophosphorus pesticides; seawater; solid phase extraction; gas chromatography; matrix effect; dichlorvos

    引用本文:彭詩琪,趙嘉輝,黃曉玲,等. 固相萃取法與GC-FPD聯用分析海水中13種有機磷[J]. 化學試劑,2022,44(2):273-278。

     

     

    基于近紅外光譜快速測定雪菊的總黃酮含量

    馮昱龍,彭娟,賀小剛,于佳萍,韓想,楚剛輝*

    (喀什大學 化學與環境科學學院 新疆特色藥食用植物資源化學實驗室,新疆 喀什844000

     

    摘要建立了一種近紅外漫反射光譜快速測定不同產地雪菊中總黃酮含量的方法。以10個不同產地的100份雪菊樣品為對象,采用NaNO2-AlNO33比色法對來自不同產地的雪菊進行總黃酮含量測定;通過不同產地雪菊樣品的近紅外光譜圖和對應的總黃酮含量,運用偏最小二乘法(PLS)建立了雪菊總黃酮含量的快速測定模型并對模型進行了驗證。試驗結果表明,采用連續小波變換與標準正態變換的方法進行光譜預處理,所建立的定量模型穩健有效,模型的相關系數為0.9862,交叉驗證均方根誤差為0.6259,預測殘差值為4.0907,預測回收率為93.06%104.64%。說明通過近紅外漫反射光譜結合化學計量學方法能夠實現快速測定不同產地雪菊中總黃酮的含量,該方法預測效果良好,結果準確,對快速、無損地測定其他植物樣品中總黃酮的含量具有一定的借鑒意義。

    關鍵詞:雪菊;近紅外光譜;總黃酮;快速測定

    中圖分類號O657.39;TQ460.7+2  文獻標識碼A     文章編號0258-32832022--

     

    Rapid Determination of Total Flavonoids in Snow Chrysanthemum Based on Near Infrared Spectroscopy Feng Yu-long, Peng Juan, He Xiao-gang, Yu Jia-ping, Han Xiang, CHU Gang-hui* (Xinjiang Special Medicine and Edible Plant Resources Chemistry Laboratory, School of Chemistry and Environmental Science, Kashgar University, Kashgar 844000, China), Huaxue Shiji, 2022, 44(2),

    Abstract: A method for the rapid determination of total flavonoids in snow chrysanthemum from different places by near-infrared diffuse reflectance spectroscopy was established. Taking 100 samples of snow chrysanthemum from 10 different producing areas as the research object, NaNO2-Al(NO3)3 colorimetric method is used to determine the total flavonoid content of snow chrysanthemum from different producing areas. Based on the near-infrared spectra and the corresponding total flavonoid content data of the snow chrysanthemum samples from different origins, a rapid determination model of snow chrysanthemum total flavonoids by using partial least squares (PLS)was established and verified. The correlation coefficient R of the established model is 0.9862, the cross validation of root mean square error RMSECV is 0.6259, the predicted residual value is 4.0907, and the predicted recovery rate is 93.06-104.64%.Therefore, the method of near-infrared diffuse reflectance spectroscopy combined with chemometrics can quickly determine the content of total flavonoids in snow chrysanthemum of different origins. This method has the advantages of good prediction effect and accurate results, and it has certain reference significance for the rapid and non-destructive determination of total flavonoids in other plant samples.

    Key words: snow chrysanthemum; near infrared spectroscopy; total flavonoids; rapid determination

    引用本文:馮昱龍,彭娟,賀小剛,等. 基于近紅外光譜快速測定雪菊的總黃酮含量[J]. 化學試劑,2022,44(2): 279-284。

     

     

    液相色譜串聯質譜與通過式固相萃取結合測定人體血液和血清中的伏立康唑和卡馬西平

     

    楊飛1,鞠華波2,劉衛3,楊進1,王穎1,鄧惠敏1,范子彥1,紀元1,唐綱嶺*1

    1. 國家煙草質量監督檢驗中心,河南 鄭州  450001;2. 西北煙草質量監督檢測站,甘肅 蘭州  730030;3. 鄭州大學 藥學院,河南 鄭州  450001

     

    摘要:采用通過式固相萃取建立高效液相色譜-串聯質譜(HPLC-MS/MS)快速測定人體血液和血清中伏立康唑和卡馬西平的方法。樣品經蛋白沉淀后過PRiME HLB通過式固相萃取柱凈化,Poroshell 120 EC-C184.6 mm×50 mm,2.7 μm)為色譜柱,0.01 mol/L醋酸銨水溶液-乙腈(含0.1%甲酸)為流動相進行梯度洗脫。在電噴霧離子源正離子模式下電離,以多反應監測模式(MRM)下掃描。同時采用基質匹配標準曲線和同位素內標法進行定量分析。結果表明:待測化合物的回收率在85.5%  106.6%之間,日內RSD和日間RSD小于10.0%,所有化合物線性關系良好(R20.9968),檢出限LOD和定量限LOQ范圍分別為0.02  0.650.07  2.12 ng/mL。該方法專屬性強、操作簡單、分離速度快、穩定性好、靈敏度高,適用于人體血液和血清中伏立康唑和卡馬西平含量的測定,為不同種類藥物的同時檢測提供了借鑒。

    關鍵詞:通過式固相萃??;卡馬西平;伏立康唑;高效液相色譜-串聯質譜

    中圖分類號:R917        文獻標識碼:A           文章編號:0258-32832022--

     

    Determination of Voriconazole and Carbamazepinein Human Blood and Serum by Liquid Chromatography Tandem Mass Spectrometry Combined with Pass-Through Solid Phase Extraction YANG Fei1, JV Hua-bo2, LIU Wei3, YANG Jin1, WANG Ying1, DENG Hui-min1, FAN Zi-yan1, JI Yuan1, TANG Gang-ling* 1 (1. China National Tobacco Quality Supervision & Test Center, Zhengzhou 450001, China; 2. North-west Tobacco Test Centre, Lanzhou 730030, China; 3. School of Pharmacy, Zhengzhou University, Zhengzhou 450001, China), Huaxue Shiji, 2022, 44(2),

    Abstract: This method established a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) for the determination of voriconazole and carbamazepine in human blood and serum by pass-through solid-phase extraction. Human whole blood/serum samples were purified by acetonitrile precipitation and PRiME HLB pass-through solid-phase extraction column. Poroshell 120 EC-C18 (4.6 mm×50 mm, 2.7 μm) was used as the chromatographic column, and0.01 mol/L ammonium acetate-acetonitrile aqueous solution (containing 0.1% formic acid)was used as the mobile phase for gradient elution. The samples were scanned in the multiple reaction monitoring (MRM) mode with positive ion mode of electrospray ionization. At the same time, the quantitative analysis of the sample was carried out using matrix matching standard curve and isotope internal standard method. The recoveries of the tested compounds were between 85.5% and 106.6%, and the intra-day relative standard deviation (RSD) and inter-day RSD were both less than 10.0%. All compounds have a good linear relationship (R2≥0.9968), while the limit of detection (LOD) and limit of quantification (LOQ) range from 0.02 to 0.65 ng/mL and 0.07 to 2.12 ng/mL, respectively. This method has strong specificity, simple operation process, fast separation speed, good stability and high sensitivity, which is suitable for the determination of voriconazole and carbamazepine in human whole blood and serum.

    Key words: pass-through solid phase extraction; carbamazepine; voriconazole; high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)

    引用本文:楊飛,鞠華波,劉衛,等. 液相色譜串聯質譜與通過式固相萃取結合測定人體血液和血清中的伏立康唑和卡馬西平[J]. 化學試劑,2022, 44(2):285-292.

     

     

    ICP-OES法測定不同水源地飲用礦泉水中35種礦物質元素

     

    貢慧1,楊震2,竇培謙1,孟燕華1,趙秋生1,任國友1,徐桂芹1

    1. 中國勞動關系學院 安全工程學院,北京  100048;2. 中國綠色食品發展中心,北京 100081)

     

    摘要:采用濕法消解為前處理方法,ICP-OES為檢測手段建立了天然飲用礦泉水中35礦物質種元素的檢測方法,優化了前處理方法,確定了35種元素的ICP-OES分析線;建立了35種元素的適合濃度范圍的標準曲線,線性相關系數均在0.995以上;檢出限在0.04 ~ 10.50 μg/L之間,定量限在0.12 ~ 35.00 μg/L之間。對35種元素的標準樣品進行了測定,相對標準偏差在0.50% ~ 8.00%之間,加標回收率在90% ~ 108%之間,方法簡便省時,精密度和準確度較高。6個水源地的天然飲用礦泉水實際樣品進行了35種礦物質元素測定,檢測結果發現天然礦泉水具有低鈉、鉀,高鈣、鎂,富有鍶、硅等有益元素的特點,但因水源地不同,各元素含量差異較大,消費者可根據自身情況加以選購。

    關鍵詞:ICP-OES;礦泉水;礦物質元素;濕法消解;不同水源地

    中圖分類號:O657.3    文獻標識碼:A      文章編號: 0258-32832022

     

    Determination of 35 Mineral Elements in Drinking Water from Different Water Sources by ICP-OES GONG Hui1*, YANG Zhen2, DOU Pei-qian1, MENG Yan-hua1, ZHAO Qiu-sheng1, REN Guo-you1, XU Gui-qin1 (1. China University of Labor Relations School of Safety Engineering, Beijing 100048, China; 2. China Green Food Development Center, Beijing 100081, China), Huaxue Shiji, 2022, 44(2),

    Abstract: The detection method of 35 mineral elements in natural drinking mineral water was established by wet digestion as pretreatment method and ICP-OES as detection method. The pretreatment method was optimized, and the ICP-OES analysis line of 35 elements was determined. The standard curves suitable for the concentration range of 35 elements were established, and the linear correlation coefficients were more than 0.995. The detection limit was 0.04-10.50 μg/L, and the quantitative limit was 0.12-35.00 μg/L. The relative standard deviation was 0.50%-8.00%, and the recovery was 90%-108%. The method was simple, time-saving and had high precision and accuracy. 35 kinds of mineral elements were determined in the actual samples of natural drinking mineral water from 6 water sources. The results showed that natural mineral water had the low ion concentration of sodium, potassium, while high ion concentration of calcium, magnesium, strontium, silicon and other beneficial elements. Notably, due to the difference in water sources, the content of each element varies greatly. In this case, consumers are suggested to choose and buy the water according to their own situation.

    Key words: ICP-OES; mineral water; mineral elements

    引用本文:貢慧,楊震,竇培謙,等. ICP-OES法測定不同水源地飲用礦泉水中35種礦物質元素[J]. 化學試劑,2022,442):293-297.

     

     

    柱串聯凝膠色譜分離表征多分散聚乙二醇羧酸衍生物的

    方法研究

     

    張安林1, 2,馬寧2,張徑*1, 2,張愛玲*1, 3

    1. 長沙創新藥物工業技術研究院有限公司,湖南 長沙  410006;2. 長沙醫學院 藥學院,湖南 長沙  410219;3. 華中科技大學同濟醫學院附屬協和醫院,湖北 武漢  430022

     

    摘要:藥用聚乙二醇(PEG)由于具有多分散特性而導致其衍生物之間的分離表征極其困難。常規的基于分子排阻(SEC)的凝膠色譜對于相同平均分子量(Mn)的PEG衍生物很難實現良好的分離效果。對平均分子量為20005000的直鏈聚乙二醇(PEG)及其羧酸衍生物進行了色譜分析。在低離子強度下,采用示差折光檢測器和3OHpark KF型色譜柱串聯對一系列多分散PEG衍生物進行了分離表征,解決了聚乙二醇及其羧酸衍生物分離表征難題。結果表明,這些PEG衍生物在OHpark KF色譜柱上的保留機制主要是離子交換相互作用。當流動相中的鹽濃度增加時,保留體積減小,并且保留體積和保留時間隨著洗脫液的溶劑比例以及柱溫的變化而變化。此外,PEG鏈的鏈長度和末端基團對PEG化合物的色譜行為也會產生明顯影響。

    關鍵詞:聚乙二醇;羧酸衍生物;分子排阻色譜;保留體積;離子交換

    中圖分類號:0626.24     文獻標識碼:A      文章編號:0258-32832022--

     

    Separation and Characterization of Polyethylene Glycol Carboxylic Acid Derivatives by Gel Chromatography with Tandem Gel Columns ZHANG An-lin1, 2, MA Ning2, ZHANG Jing*1, 2, ZHANG Ai-ling*1, 3  (1. Changsha Institute of Innovative Pharmaceutical Industry Technology, Changsha 410006, China; 2. School of Pharmacy, Changsha Medical College, Changsha 410219, China; 3. Union Hospital, Tongji Medical College, Huazhong University of Science and Technology, Wuhan 430022, China), Huaxue Shiji, 2022, 44(2),

    Abstract: Due to the polydispersion characteristics of medicinal polyethylene glycol (PEG), it is extremely difficult to separate and characterize PEG derivatives. Conventional gel chromatography based on size exclusion chromatography (SEC) is difficult to achieve a good separation effect for PEG derivatives with the same average molecular weight (Mn). This research describes achromatographic analysis of straight-chain polyethylene glycol (PEG) and their carboxyl-substituted derivatives (Mn=2000 or 5000). A series of polydisperse PEG derivatives were separated by tandem OHpark KF column under low ionic strength with refractive index detection (RID). The problem inseparation and characterization of carboxylic functionalized and unfunctionalized polyethylene glycol (PEG) due to its polydispersion property was solved. The results showed that the retention mechanism of these PEG derivatives on the OHpark KF column was mainly the ion exchange interactions, because the retention volume decreased with the increase of salt concentration in the mobile phase, and the retention time and volume changed with the solvent content and column temperature. Moreover, the size and the end functional groups of the PEG chain also have an obvious effect on the chromatographic behavior of PEG compounds.

    Key words: poly(ethyleneglycol); carboxylic acid derivatives; size-exclusion chromatography; retention volume; ion exchange

    引用本文:張安林,馬寧,張徑,等. 柱串聯凝膠色譜分離表征多分散聚乙二醇羧酸衍生物的方法研究[J]. 化學試劑,2022,44(2)298-305.

     

     

    電感耦合等離子體串聯質譜法測定高純氧化釓中20種痕量元素含量

    胡芳菲*1,劉鵬宇2,于磊1,王長華1,陳雄飛1

    (1. 國標(北京)檢驗認證有限公司,北京 101407 ;2. 國合通用測試評價認證股份公司,北京 101407)

    摘要建立了電感耦合等離子體串聯質譜法(ICP-MS/MS)直接測定高純氧化釓中20種痕量元素含量的分析方法。在優化的實驗條件下,分別采用He碰撞模式NH3原位質量模式消除了Fe、As、Yb、Lu受到的質譜干擾,考察了基體效應以及不同內標元素的校正效果,方法定量限在0.0030.63 μg/g之間,RSDn=75%,加標回收率在90%115%之間。本方法可以用于高純氧化釓中包括YbLu在內的痕量元素含量的直接測定。

    關鍵詞電感耦合等離子體串聯質譜;氧化釓;痕量元素;鐿;镥

    中圖分類號:O657.63      文獻標識碼:A      文章編號:0258-32832022--

     

    Determination of 20 trace elements in high purity gadolinium oxide by inductively coupled plasma-tandem mass spectrometry HU Fang-fei*1, LIU Peng-yu2, YU Lei1, WANG Chang-hua1, CHEN Xiong-fei1 (1.Guobiao(Beijing) Testing & Certification Co., Ltd.; 2. China United Test & Certification Co., Ltd., Beijing 101407, China), Huaxue Shiji, 2022, 44(2),

    Abstract: An analytical method was proposed to determine 20 impurity elements in high pure gadolinium oxide by inductively coupled plasma-tandem mass spectrometry. This work was finished under optimal conditions. He collision mode and NH3 in-situ mass mode were used to eliminate mass interference of Fe, As, Yb and Lu contents. Matrix effect and correction results of different internal standards were investigated. The limits of quantitation for each element were 0.0030.63 μg/g, and the relative standard deviation (RSD, n=7) was below 5%. The recoveries for the testing spiked samples were between 90% and 115%. This method can be used to measure trace element contents in high purity gadolinium oxide directly, including Yb and Lu.

    Key words: inductively coupled plasma-tandem mass spectrometry; gadolinium oxide; trace elements; Ytterbium; Lutetium

    引用本文胡芳菲,劉鵬宇,于磊,等. 電感耦合等離子體串聯質譜法測定高純氧化釓中20種痕量元素含量[J]. 化學試劑,2022,44(2): 306-309。

     

     

    氮雜環基取代丙氨酸及其衍生物的合成、晶體結構及熒光性能研究

    雷紅琴1,2,王吉德*1,史岷山1

    1. 新疆大學 石油天然氣精細化工教育部重點實驗室,新疆 烏魯木齊  830046;2. 伊寧海關技術中心, 新疆 伊寧 835000

     

    摘要采用2-(二苯亞甲氨基)乙酸甲酯和32-/4-溴甲基取代的含氮雜環化合物分別進行烷基化、水解反應得到了3-(1H-苯并[d]咪唑-2-)-2-氨基丙酸、3- (吡啶-2-)-2-氨基丙酸及3-(噻唑-4-)-2-氨基丙酸。所合成化合物的結構經過元素分析、1HNMR、13CNMR、IR和質譜確認,并用X射線衍射法測定了化合物2-(二苯亞甲氨基)-3-(1-叔丁氧羰基-1H-苯并[d]咪唑-2-)丙酸甲酯及 2-(二苯亞甲氨基)-3-(噻唑-4-)丙酸甲酯晶體結構。同時測試了標題化合物及其前體化合物的熒光性質,通過測試發現上述幾種化合物具有很強的熒光,增大了其作為熒光材料的應用可能性。

    關鍵詞雜芳基氨基酸;烷基化;合成;熒光性能;晶體結構

    中圖分類號:O625.63    文獻標識碼:A       文章編號:0258-3283(2022)--

     

    Synthesis, Crystal Structure and Fluorescent property of Several N-Containing Heteroaromatic Amino Acids and Derivatives LEI Hong-qin1,2,WANG Ji-de*1, SHI Min-shan1 (1. Key Laboratory of Oil and Gas Fine Chemicals, Ministry of Education & Xinjiang Uyghur Autonomous Region, Xinjiang University, Urumqi 830046, China; 2 Yining Customs Technical Centre, Yining  835000, China), Huaxue Shiji, 2022, 44(2),

    Abstract; 2-amino-3-(1H-benzo[d]imidazol-2-yl)propanoic acid, 2-amino-3-(pyridin-2-yl) propanoic acid and 2-amino-3- (thiazol-4-yl)propanoic acid have been synthesized by alkylation of N-(diphenyl methylene) glycine methyl ester with 3 kinds of nitrogen containing heterocycles and hydrolization subsequently. The target compounds were characterized by elemental analysis, 1H NMR, 13C NMR, IR, MS technique.Moreover, the crystal structures of methyl 2-(diphenylmethyleneamino)-3-(1 -tert-butoxycarbonyl-1H-benzo[d]imidazol-2-yl)propanoate and methyl 2-(diphenylmethyleneamino)-3-(thiazol-4-yl)propanoate were also determined by X-ray diffraction.Besides, we found that these compounds have strong fluorescence, which increases their potential application as fluorescent materials.

    Key words: heteroaromatic amino acids; alkylation; synthesis; fluorescent property; crystal structure

    引用本文:雷紅琴, 王吉德, 史岷山. 氮雜環基取代丙氨酸及其衍生物的合成、晶體結構及熒光性能研究[J].化學試劑,2021,44(2)310-316.

     


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