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您的位置:中国色谱网 >> 资讯 >> 技术应用 >> 图书期刊 >> 《色谱》2012年第12期内容摘要
《色谱》2012年第12期内容摘要
2012年12月25日 来源:中国色谱网 责编:李华静

1211-1213

DOI: 10.3724/SP.J.1123.2012.11018

收稿日期: 2012-11-26

*通讯联系人: 汪其,中国科学院大连化学物理研究所图书馆馆长,研究馆员,兼任大连市科技情报学会理事。

收稿日期:2012-11-26

 

从文献计量学角度看色谱研究现状和发展趋势

汪其

(中国科学院大连化学物理研究所, 辽宁 大连 116023)

摘要: 分析化学是研究物质的组成、结构、形态等化学信息的分析方法和理论的一门科学,在科学研究中发挥着重要作用。分析化学中的色谱研究作为一种分析方法,起源于20世纪初,随着现代色谱研究水平的不断提高和技术的不断发展,已得到越来越广泛的应用。本文通过美国科学信息研究所(ISI)的Web of Science 数据库(即SCI-E)检索色谱(包括毛细管电泳)研究论文数据,进行国家间、机构间的分析对比,从而了解色谱研究现状和发展趋势,为学科研究规划布局提供参考。

 

1214-1219

DOI: 10.3724/SP.J.1123.2012.12001

*通讯联系人: 屈锋,博士,教授,博士生导师,研究方向为生物医药分析检测. Tel: (010)68918015, E-mail: qufengqu@bit.edu.cn.

基金项目: 国家自然科学基金项目(21175011, 20875009)和科技部基础研究计划项目(2012CB910603).

收稿日期: 2012-12-03

 

2012年毛细管电泳技术年度回顾

屈锋1*, 赵新颖1,2, 王勇1

(1. 北京理工大学生命学院, 北京 100081; 2. 北京市理化分析测试中心, 北京 100089)

摘要: 本文为2012年毛细管电泳(CE)技术的年度回顾。文中介绍了2012年涉及CE技术的国际会议4个,国内会议3个,对各会议的研究报道进行了总结。文中还归纳了ISI Web of Science中检索的2012年度发表的CE论文,并对这些CE论文在生物医药研究和检测器使用以及重要分析化学杂志发表的情况进行了分类说明。

关键词: 毛细管电泳;2012年;年度回顾

文章编号: 1000-8713(2012)12-1214-06

 

2012 annual review of capillary electrophoresis technology

QU Feng1*, ZHAO Xinying1,2, WANG Yong1

(1. School of Life Science, Beijing Institute of Technology, Beijing 100081, China; 2. Beijing Centre for Physical and Chemical Analysis, Beijing 100089, China)

Abstract: This paper reviews the capillary electrophoresis (CE) in 2012. Four international and three national conferences are included and the important reports are introduced briefly. Literatures searched from ISI Web of Science ranged in 2012.1.1~2012.12.1 are classified and introduced based on the biology and medicine applications as well as the use of detectors and the important analytical chemical journals.

Key words: capillary electrophoresis (CE); 2012; annual review

 

1220-1228

DOI: 10.3724/SP.J.1123.2012.08002

*通讯联系人: 李攻科,教授,研究方向为色谱分析、复杂体系分离分析. Tel: (020)84110922, E-mail: cesgkl@mail.sysu.edu.cn.

基金项目: 国家自然科学基金项目(21127008, 21075140, 21105133和91232703)、高等学校博士学科点专项科研基金项目(20120171110001)、国家重大科学仪器设备开发专项项目(2011YQ03012409)、广东省科技计划项目(2010B090400142)和广州市科技计划项目(12A102051514).

收稿日期: 2012-08-01

 

分子印迹微萃取技术的研究进展

张凯歌, 胡玉玲, 胡玉斐, 李攻科*

(中山大学化学与化学工程学院, 广东 广州 510275)

摘要: 微萃取技术是一种将分析物高效萃取富集于微体积的聚合物或有机溶剂中,集采样、萃取、浓缩、进样于一体的无(少)溶剂、易于与其他技术在线联用的样品前处理方法。分子印迹聚合物是一种具有强大分子识别功能的材料,具有高效的选择特异性,可从复杂样品中选择性分离富集目标分析物,在微萃取技术中得到了广泛的应用。本文综述了近年来分子印迹微萃取技术的研究进展,包括分子印迹固相微萃取、分子印迹搅拌棒吸附萃取、分子印迹磁性微球萃取等微萃取技术。共引用文献75篇。

关键词: 分子印迹微萃取;分子印迹固相微萃取;分子印迹搅拌棒吸附萃取;分子印迹磁性微球萃取;综述

文章编号: 1000-8713(2012)12-1220-09

 

Development of molecularly imprinted microextraction techniques

ZHANG Kaige, HU Yuling, HU Yufei, LI Gongke*

(School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275, China)

Abstract: Microextraction techniques can extract efficiently the analytes from a sample matrix to the polymers or organic solvents of microvolume, and integrate sampling, extraction, concentration and injection into one single step. They have the advantages of simple, time-efficient and solvent-free. They have been successfully coupled with a variety of analytical tools, such as gas chromatography and high performance liquid chromatography. Molecularly imprinted polymers have specific recognition ability. They can separate and enrich analytes from complicated matrix with high selectivity, and they have great application prospects in complicated sample preparation. This review summarizes the progress in the molecularly imprinted microextraction techniques, including molecularly imprinted-solid phase microextraction, molecularly imprinted-stir bar adsorptive extraction, magnetic molecularly imprinted beads extraction, etc. A total of 75 references are cited.

Key words: molecularly imprinted microextraction; molecularly imprinted-solid phase microextraction; molecularly imprinted-stir bar adsorptive extraction; magnetic molecularly imprinted beads extraction; review

 

1229-1234

DOI: 10.3724/SP.J.1123.2012.09033

*通讯联系人: 屈锋,博士,教授,博士生导师,主要研究方向为生物医药分析检测. E-mail: qufengqu@bit.edu.cn.#并列第一作者.

基金项目: 国家自然科学基金项目(21175011, 20875009)、科技部基础研究计划项目(2012CB910603)和“十二五”国家科技支撑计划项目(2011BAD26B0404).

收稿日期: 2012-09-20

 

毛细管电泳法评价细胞色素c与单链脱氧核糖核酸库的相互作用

梅芳1, 赵新颖1,2#, 屈锋1*

(1. 北京理工大学生命学院, 北京 100081; 2. 北京市理化分析测试中心, 北京 100089)

摘要: 以细胞色素c(Cyt c)为碱性蛋白质模型,建立了毛细管电泳评价Cyt c与3种不同链长的单链脱氧核糖核酸(ssDNA)库相互作用的评价方法,研究了离子强度对Cyt c与ssDNA库相互作用的影响。比较了Cyt c与含有20、40和60个随机碱基序列的3种不同链长的ssDNA库的作用及基于未涂层毛细管和涂层毛细管的毛细管区带电泳方法。因碱性蛋白质在未涂层毛细管管壁上存在吸附,因此利用未涂层毛细管区带电泳不能区别3种ssDNA库与其作用的差异。利用涂层毛细管电泳法,在压力辅助的反向电压下,根据游离ssDNA库的峰面积变化可比较3种ssDNA库与细胞色素c的相互作用差异。结果表明,含有20个随机寡核苷酸链长的ssDNA库与Cty c的作用最强。此外,NaCl浓度显著影响Cyt c与ssDNA60库的作用。在优化的实验条件下,0.02 mol/L NaCl有利于两者的相互作用。调节盐浓度可抑制非特异性静电作用,能提高碱性蛋白质适配体的单轮筛选效率。利用未涂层毛细管电泳分析复合物及游离ssDNA库的峰面积变化,可优化有利复合物形成的盐浓度。

关键词: 毛细管电泳;细胞色素c;单链DNA库;碱性蛋白质;核酸适配体

文章编号: 1000-8713(2012)12-1229-06

 

Comparison of interaction between cytochrome c and single strain deoxyribonucleic acid pools based on capillary electrophoresis

MEI Fang1, ZHAO Xinying1,2, QU Feng1*

(1. School of Life Science, Beijing Institute of Technology, Beijing 100081, China; 2. Beijing Centre for Physical and Chemical Analysis, Beijing 100089, China)

Abstract: An assessment method of the interaction between cytochrome c (Cyt c) selected as a representative basic protein and three lengths of single strain deoxyribonucleic acid (ssDNA) pools was presented based on capillary electrophoresis. The investigation of ionic strength effect on the interaction was made. The interactions between Cyt c and the ssDNA pools with 20 nt, 40 nt and 60 nt random sequences were compared by capillary zone electrophoresis (CZE) based on an uncoated fused capillary and a coated capillary. Using the uncoated fused capillary, the interaction difference could not be observed due to the strong adsorption of Cyt c on the inner surface of the capillary. However, under negative potential with the assistance of pressure driving, the peak area change of free ssDNA indicated the interaction difference of the three pools with Cyt c using the coated capillary, and the results showed that the ssDNA pool with 20 nt random sequence exhibited the strongest interaction. In addition, NaCl concentration had great effect on the interaction of Cyt c with ssDNA60, and 0.02 mol/L NaCl solution was favored. For the selection of basic target proteins, the adjustment of salt concentration would inhibit the non-specific electrostatic interaction, improve the selection efficiency of a selection round. The favorable salt concentration could be optimized with an uncoated fused capillary by comparing the peak area change of the complex and free ssDNA pool.

Key words: capillary electrophoresis (CE); cytochrome c; ssDNA pool; basic protein; aptamer

 

1235-1240

DOI: 10.3724/SP.J.1123.2012.09001

*通讯联系人: 刘芃岩,博士,教授,主要研究方向为食品及环境污染物分析. E-mail: pyliu01@yahoo.com.cn.

基金项目: 河北省教育厅重点项目(ZH200805)和保定市科技局项目(08J03).

收稿日期: 2012-09-03

 

食品包装材料中7种光引发剂向水性模拟液中的迁移测定

刘芃岩*, 黄恩洁, 陈艳杰

(河北大学化学与环境科学学院, 河北 保定 071002)

摘要: 为了考察食品包装材料中光引发剂向食品中迁移的情况,以水性模拟液作为迁移溶剂,用65 μm聚二甲基硅氧烷/二乙烯基苯(PDMS-DVB)纤维头进行固相微萃取结合气相色谱-质谱(SPME/GC-MS)分析方法同时测定食品包装材料中7种光引发剂(PIs)的迁移量。方法的检出限为0.0012-0.0069 μg/L,线性范围为0.03-1.0 μg/L (r2>0.9909),在3种浓度的添加水平下,加标回收率为70.8%-112.0%,相对标准偏差不大于14.0%。利用建立的方法对20个实际样品进行测定,发现所有样品中均检出二苯甲酮,其中10个样品中检出4-甲基二苯甲酮,3个样品中检出1-羟基环己基苯基甲酮,1个样品中检出安息香双甲醚。该方法的灵敏度高,样品前处理过程简单,无需使用有机溶剂,为食品接触材料表面印刷油墨中PIs向水性样品中的迁移测定提供了参考。

关键词: 固相微萃取;气相色谱-质谱;光引发剂;食品包装材料;水性食品模拟液;迁移

文章编号: 1000-8713(2012)12-1235-06

 

Determination of the migration of seven photoinitiators in food packaging materials into aqueous solvent

LIU Pengyan*, HUANG Enjie, CHEN Yanjie

(College of Chemistry & Environmental Science, Hebei University, Baoding 071002, China)

Abstract: The quantity of photoinitiators (PIs) migrated into hydrosoluble foods from packaging materials is usually very small. It is hardly detectable by using the current methods. For this reason, the article describes a new effective method for detecting the migration of PIs. In this method, the migration experiment was done in aqueous food simulation. After the PIs in printing inks used in food contact materials were extracted from the solution via solid-phase microextraction (SPME) using 65 μm polydimethylsiloxane/divinylbenzene (PDMS-DVB)-coated fiber, their migration amounts were determined by gas chromatography-mass spectrometry (GC-MS) in the selected ion monitoring mode (SIM). The PIs determined by SPME/GC-MS were benzophenone (BP), 1-hydroxycyclohexyl-phenylketone (CPK), ethyl-4-dimethyl-aminobenzoate (EDMAB), 4-methylbenzophenone (4-MBP), 2,2-dimethoxy-2-phenylacetophenone (2,2-DMPA), methyl 2-benzoylbenzoate (OMBB) and 2-ethylhexyl-4-dimethyl-aminobenzoate (EHDAB). The limits of detection (S/N=3) were between 0.0012 and 0.0069 μg/L. The linearity ranged from 0.03 to 1.0 μg/L (r2>0.9909). The recoveries were in the range from 70.8% to 112.0% (n=3) with the relative standard deviations no more than 14.0%. Twenty samples were tested by using this developed method. The analytical results showed that BP was detected in all samples, and the migration amounts of BP were from 0.002 to 0.074 μg/dm2; 4-MBP was detected in ten samples, and the migration amounts of 4-MBP were from 0.006 to 0.019 μg/dm2; CPK was detected in three samples, and its amounts were 0.005, 0.005, 0.007 μg/dm2; 2,2-DMPA was detected as 0.009 μg/dm2 in one sample. The determination of real samples showed this method is feasible. The method is sensitive, simple and free from organic solvents. It could make reference to migrating determination of PIs in printing inks on food packaging surface.

Key words: solid-phase microextraction (SPME); gas chromatography-mass spectrometry (GC-MS); photoinitiators; food-packaging material; aqueous food simulant; migration

 

1241-1245

DOI: 10.3724/SP.J.1123.2012.08020

*通讯联系人: 王炳玲,博士,讲师. Tel: (025)86862748, E-mail: blwang@njmu.edu.cn.

基金项目: 国家自然科学基金面上项目(81072268)、江苏省自然科学基金面上项目(BK2010535)、江苏省博士后基金项目(1001017C)和江苏高校优势学科建设工程资助项目.

收稿日期: 2012-08-14

 

超声辅助萃取-气相色谱-负化学电离源质谱法测定室内灰尘样品中8种常见多溴联苯醚

张晓玲1, 王炳玲2*, 陆晓梅1, 张琦2, 张正东2

(1. 南京医科大学公共卫生学院卫生检验学系, 江苏 南京 210029; 2. 南京医科大学公共卫生学院职业医学与环境卫生学系, 江苏 南京 210029)

摘要: 建立了室内灰尘样品中8种常见多溴联苯醚(PBDEs: BDE-28、BDE-47、BDE-99、BDE-100、BDE-153、BDE-154、BDE-183和BDE-209)的气相色谱-负化学电离源质谱(GC-NCI/MS)分析方法。样品经吸尘器采集、正己烷超声萃取、浓缩后,采用GC-NCI/MS测定。结果表明,方法的加标回收率为53.2%-107.6%,日内测定的相对标准偏差(RSD)为2.8%-16.5%,日间测定的RSD为6.4%-22.6%。除了BDE-209的检出限(信噪比为3)为0.15 ng/g外,其他多溴联苯醚的检出限为0.003-0.015 ng/g。该方法灵敏度高,准确度和精密度好,简便快速,溶剂消耗量少,适用于灰尘中三溴-十溴联苯醚的测定。

关键词: 超声辅助萃取;气相色谱-负化学电离源质谱;多溴联苯醚;室内灰尘

文章编号: 1000-8713(2012)12-1241-05

 

Determination of polybrominated diphenyl ethers in indoor dust using ultrasonic-assisted extraction and gas chromatography-negative chemical ionization mass spectrometry

ZHANG Xiaoling1, WANG Bingling2*, LU Xiaomei1, ZHANG Qi2, ZHANG Zhengdong2

(1. Department of Hygienic Analysis and Detection, School of Public Health, Nanjing Medical University, Nanjing 210029, China; 2. Department of Occupational Medicine and Environmental Health, School of Public Health, Nanjing Medical University, Nanjing 210029, China)

Abstract: A method for the determination of eight polybrominated diphenyl ethers (PBDEs) in indoor dust was developed. A vacuum cleaner was used for gathering the house dust, and n-hexane was added and the extraction was performed in an ultrasonic bath. The supernatant was concentrated and then n-hexane was added to 0.1 mL. Gas chromatography-negative chemical ionization mass spectrometry (GC-NCI/MS) has been investigated for the determination of the eight PBDE congeners in indoor dust. The eight PBDEs were separated within 20 min. The absolute recoveries were 53.2%~107.6%. The relative standard deviations (RSDs) of intra-day were between 2.8% and 16.5%, while the RSDs of inter-day were between 6.4% and 22.6%. The limits of detection (LOD, S/N=3) were in the range of 0.003~0.015 ng/g except the LOD of BDE-209 was 0.15 ng/g. The results indicated that the proposed method is sensitive, accurate, fast, simple, low solvent consumption and suitable for the determination of tri- to deca-BDEs in indoor dust.

Key words: ultrasonic-assisted extraction; gas chromatography-negative chemical ionization mass spectrometry (GC-NCI/MS); polybrominated diphenyl ethers (PBDEs); indoor dust

 

1246-1252

DOI: 10.3724/SP.J.1123.2012.07014

*通讯联系人: 丁涛,硕士,高级工程师,研究方向为食品安全. Tel: (025)52345187, E-mail: dingt@jsciq.gov.cn.

基金项目: 国家质检总局项目(2011IK218和201010073-04).

收稿日期: 2012-07-09

 

高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速检测6种农产品中96种农药的残留量

吴斌, 丁涛*, 柳菡, 陈惠兰, 赵增运, 张睿, 沈崇钰

(江苏出入境检验检疫局动植物与食品检测中心, 江苏 南京 210001)

摘要: 利用高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速筛选辣椒、青花菜、脱水土豆、大豆、绿茶和大蒜中96种农药残留。样品经含0.1%醋酸的乙腈提取,分散固相萃取脱水、除色、净化后,以C18色谱柱为分析柱,甲醇和5 mmol/L醋酸铵水溶液作为流动相进行梯度洗脱分离。采用正、负离子切换同时测定96种农药残留,大大提高了检测通量。通过优化分辨率,在全扫描模式下提取目标化合物的精确质量数,有效地去除了基质干扰;采用自动触发采集二级质谱图进一步提高了定性的准确性。在1-200 μg/L范围内,96种农药的线性相关系数均大于0.99。通过实际样品的添加回收试验,回收率范围为58%-105%,相对标准偏差为8.8%-18.3%。该方法的检测低限可以达到5 μg/kg,可以作为蔬菜中多种农药残留高通量筛选和确认检测方法。

关键词: 高效液相色谱;静电场轨道阱;高分辨质谱;农药残留;农产品

文章编号: 1000-8713(2012)12-1246-07

 

Fast screening ninety-six pesticides in six kinds of agricultural products by high performance liquid chromatography-quadrupole/electrostatic field orbit trap high-resolution mass spectrometry

WU Bin, DING Tao*, LIU Han, CHEN Huilan, ZHAO Zengyun, ZHANG Rui, SHEN Chongyu

(Animal, Plant and Food Inspection Center of Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China)

Abstract: A high-throughput method for the determination of 96 pesticides in six kinds of agricultural products by liquid chromatography-quadrupole/electrostatic field orbit trap high-resolution mass spectrometry was developed. After extraction with 0.1% acetic acid in acetonitrile solution and concentration, dispersive solid-phase extraction was further utilized to reduce the matrix interference. The chromatographic analysis was performed on a C18 column with methanol and 5 mmol/L ammonium acetate solution as the mobile phases with a gradient elution program. The 96 pesticide residues were analyzed in switching positive and negative modes at the same time. With the optimized mass resolution, accurate mass-to-charge ratio extraction of the target pesticide compounds in full scan mode could eliminate matrix interference effectively. Two-stage threshold-triggered full mass scan mode was utilized to further improve the accuracy of qualitative analysis. The linear ranges of all the 96 pesticides were from 1 μg/L to 200 μg/L with correlation coefficients greater than 0.99. By detecting spiked samples, the detection limits were 5 μg/kg for all the residues and the recoveries were in the range of 58%~105% with the relative standard deviations (RSDs) between 8.8% and 18.3%.

Key words: high performance liquid chromatography (HPLC); electrostatic field orbit trap; high-resolution mass spectrometry; pesticide residues; agricultural products

 

1253-1259

DOI: 10.3724/SP.J.1123.2012.07038

*通讯联系人: 刘正才,高级工程师,主要从事农兽药残留分析. E-mail: zhengcailiu@yahoo.com.cn.

基金项目: 国家质检总局科技项目(2010IK183)和福建省科技攻关重点项目(2010Y0001).

收稿日期: 2012-07-26

 

液相色谱-电喷雾串联质谱法同时检测鸡组织中5种抗病毒类药物的残留量

刘正才*, 杨方, 余孔捷, 林永辉, 刘素珍, 张琼, 苏芝娇

(福建出入境检验检疫局, 福建 福州 350001)

摘要: 建立了鸡组织中抗病毒类药物多残留检测的液相色谱-电喷雾串联质谱法(LC-ESI-MS/MS)。采用三氯乙酸-乙腈溶液提取鸡组织中的金刚烷胺、金刚乙胺、美金刚、咪喹莫特和吗啉胍,离心过滤后经强阳离子交换柱(SCX)净化,色谱柱Xamide(100 mm×2.1 mm, 5 μm)分离,多反应监测(MRM)正离子扫描方式进行质谱检测。结果表明,鸡组织与鸡肝中5种药物的检出限为0.06-0.30 μg/kg,定量限为0.2-1.0 μg/kg。当5种药物的添加水平为0.2-10.0 μg/kg时,在鸡肉中的平均回收率为72.3%-94.2%,相对标准偏差(RSD)(n=6)为3.5%-11.3%;在鸡肝中的平均回收率为70.8%-92.7%, RSD(n=6)为5.3%-12.6%。该方法选择性好,抗干扰能力强,可作为鸡肉和鸡肝中抗病毒药物残留检测的确证方法。

关键词: 液相色谱-电喷雾串联质谱法;抗病毒类药物;鸡肉;鸡肝;多残留检测

文章编号: 1000-8713(2012)12-1253-07

 

Multi-residue determination of five antiviral drugs in chicken tissues by liquid chromatography-electrospray ionization tandem mass spectrometry

LIU Zhengcai*, YANG Fang, YU Kongjie, LIN Yonghui, LIU Suzhen, ZHANG Qiong, SU Zhijiao

(Fujian Entry-Exit Inspection & Quarantine Bureau, Fuzhou 350001, China)

Abstract: A method of liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) for the simultaneous determination of five antiviral drug residues, amantadine, rimantadine, memantine, moroxydine and imiquimod in chicken tissues was developed. The compounds were extracted from the samples with trichloroacetic acid solution and acetonitrile, and then cleaned-up by strong cation exchange (SCX) solid phase extraction cartridges. The analytes were separated on a Xamide column (100 mm×2.1 mm, 5 μm) and determined qualitatively and quantitatively with tandem mass spectrometry using positive polarity mode under multi-reaction monitoring (MRM) scan type. The limits of detection and the limits of quantification were 0.06~0.30 μg/kg and 0.2~1.0 μg/kg, respectively. The average recoveries of the five drugs were 72.3%~94.2% in chicken muscle and 70.8%~92.7% in chicken livers. The relative standard deviations (RSDs) in chicken muscle and livers were 3.5%~11.3% and 5.3%~12.6%, respectively. The method is selective without interference and suitable for the determination and confirmation of the five antiviral drugs in chicken muscle and livers.

Key words: liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS); antiviral drugs; chicken muscle; chicken livers; multi-residue determination

 

1260-1264

DOI: 10.3724/SP.J.1123.2012.07031

*通讯联系人: 林永辉,硕士,工程师. Tel: (0591)87065541, E-mail: xmulyh@163.com.

基金项目: 国家质量监督检验检疫总局科研项目(2009IK143)和福建检验检疫局科技计划项目(FK2011-35).

收稿日期: 2012-07-17

 

柱前衍生化液相色谱-串联质谱法测定茶叶中草铵膦的残留量

林永辉*, 刘正才, 杨方, 邱元进, 刘素珍, 苏芝娇, 张琼, 薛芝敏, 方宇

(福建出入境检验检疫局, 福建 福州 350001)

摘要: 建立了茶叶中草铵膦残留检测的液相色谱-串联质谱分析方法。样品经水超声提取,C18固相萃取小柱净化,9-芴基氯甲酸酯(FMOC-Cl)溶液在硼酸盐缓冲溶液下衍生2 h后,用Kinetex C18色谱柱分离,以乙腈和5 mmol/L乙酸铵水溶液(含0.2%(v/v)甲酸)作为流动相进行梯度洗脱,电喷雾负离子模式电离(ESI~),多反应监测(MRM)模式检测,外标法定量。方法的线性范围为2.5-50.0 μg/L,相关系数r2大于0.999;定量限为0.10 mg/kg。在不同基质中,草铵膦在0.10、0.50、1.00 mg/kg添加水平下的平均回收率为61.6%-81.4%,相对标准偏差为3.2%-8.4%。该方法具有快速简便、灵敏度高、准确性强等特点,适用于茶叶中草铵膦残留量的检测。

关键词: 柱前衍生;液相色谱-串联质谱;草铵膦;茶叶

文章编号: 1000-8713(2012)12-1260-05

 

Determination of glufosinate residue in tea by liquid chromatography-tandem mass spectrometry coupled with precolumn derivatization

LIN Yonghui*, LIU Zhengcai, YANG Fang, QIU Yuanjin, LIU Suzhen, SU Zhijiao, ZHANG Qiong, XUE Zhimin, FANG Yu

(Fujian Entry-Exit Inspection and Quarantine Bureau, Fuzhou 350001, China)

Abstract: A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was established for the determination of glufosinate (GLUF) residue in tea. The GLUF was extracted with water for 30 min under ultrasonication, and cleaned-up using a C18 solid phase extraction cartridge, then derived using fluorenylmethylchloroformate (FMOC-Cl) in borate buffer for 2 h. The separation was performed on a Kinetex C18 column with the mobile phases of acetonitrile and 5 mmol/L ammonium acetate aqueous solution (containing 0.2% (v/v) formic acid) in a gradient elution mode. The identification and quantification of the GLUF were carried out by MS/MS in negative electrospray ionization (ESI~) and multiple reaction monitoring (MRM) mode, the quantification analysis was performed by external standard method. The calibration curve showed good linearity in the range of 2.5~50.0 μg/L with the correlation coefficient r2>0.999. The limit of quantification (LOQ) was 0.10 mg/kg. The average recoveries of GLUF spiked at 0.10, 0.50 and 1.00 mg/kg levels in tea were between 61.6% and 81.4%, and the relative standard deviations (RSDs) were between 3.2% and 8.4%. The method is simple, rapid, sensitive, accurate and suitable for the confirmation and quantification of GLUF in tea.

Key words: precolumn derivatization; liquid chromatography-tandem mass spectrometry (LC-MS/MS); glufosinate; tea

 

1265-1270

DOI: 10.3724/SP.J.1123.2012.07035

*通讯联系人: 范华均,博士,教授,主要从事药物提取分离及药物分析. E-mail: junhuafan@126.com.

基金项目: 国家“重大新药创制”科技重大专项(2011ZX09102-001-31)和广东药学院师资队伍建设基金项目(52104109).

收稿日期: 2012-07-21

 

几种苯甲酰胺类抗精神病药物的手性色谱拆分及其对映体含量的测定

王李平, 范华均*, 巫坤宏, 彭晓升, 江子滔, 臧林泉

(广东药学院药科学院, 广东 广州 510006)

摘要: 采用直链淀粉-三(5-氯-2-甲基苯基氨基甲酸酯)手性固定相(CSP),以0.1%二乙胺正己烷和0.1%二乙胺乙醇为流动相梯度洗脱,以舒必利、阿米舒必利和莫沙必利为目标物,利用高效液相色谱法研究了这3种苯甲酰胺类药物的手性色谱分离行为。分别考察了流动相组成、添加剂及柱温对3种药物对映体分离的影响,从热力学和结构上探讨了色谱拆分的机理。结果表明: 在优化的色谱条件下,舒必利、阿米舒必利和莫沙必利对映体的分离度Rs>1.5;计算了3种药物对映体的色谱保留因子k和分离因子α,以及与CSP相互作用的热力学函数,其相互作用大小依次为舒必利>阿米舒必利>莫沙必利。已将该方法成功地应用于上述3种药物片剂和血清中其对映体的测定,方法简便、准确、可靠。

关键词: 高效液相色谱法;舒必利;阿米舒必利;莫沙必利;药物;手性拆分

文章编号: 1000-8713(2012)12-1265-06

 

Chiral separation of benzamide antipsychotics and determination of their enantiomers by high performance liquid chromatography

WANG Liping, FAN Huajun*, WU Kunhong, PENG Xiaosheng, JIANG Zitao, ZANG Linquan

(College of Pharmacy, Guangdong Pharmaceutical University, Guangzhou 510006, China)

Abstract: A new method of the chiral separation of three drugs such as sulpiride, amisulpride and mosapride was developed on the chiral stationary phase of amylose-tris-(5-chloro-2-methyl- phenylcarbamate) (ACMPC) by high performance liquid chromatography. The chromatographic behaviors of enantiomers of the three drugs were investigated in the mobile phases consisted of ethanol and n-hexane (containing 0.1%(v/v) diethylamine). The chromatographic conditions including the composition of the mobile phase, additives and temperature were further optimized for the chiral separation. The mechanism of racemic resolution for the mentioned drugs is discussed thermodynamically and structurally. The results indicated that these three chiral drugs could be separated on an ACMPC column under the optimum conditions, and their chiral resolutions were improved up to more than 1.5. The chromatographic parameters such as the retention factor k, separation factor α are presented, and the thermodynamic functions were calculated for the separation of the enantiomers of the three drugs. The method has been successfully applied to the determination of the enantiomers of the three drugs in tablets and blood serum. It is simple, reliable and accurate.

Key words: high performance liquid chromatography (HPLC); sulpiride; amisulpride; mosapride; drugs; chiral separation

 

1271-1275

DOI: 10.3724/SP.J.1123.2012.07024

*通讯联系人: 彭缨,副教授,主要研究方向为中药药效物质基础及质量控制研究. E-mail: yingpeng1999@yahoo.com.cn.

基金项目: 辽宁省博士启动基金项目(20111139)和辽宁省高等学校杰出青年学者成长计划资助项目(LJQ2011105).

收稿日期: 2012-07-17

 

高效液相色谱法考察不同炮制方法对知母中5种主要化学成分的影响

赵路路1, 刘菲菲1, 彭缨1,2*, 康廷国2

(1. 沈阳药科大学中药学院, 辽宁 沈阳 110016; 2. 辽宁中医药大学, 辽宁 沈阳 110032)

摘要: 建立了高效液相色谱(HPLC)同时测定知母不同炮制品中新芒果苷、芒果苷、知母皂苷BIII、知母皂苷I和知母皂苷AIII含量的方法,探讨了不同炮制方法对知母化学成分的影响,为通过采用不同炮制方法来改变知母药性提供了依据。采用AlltimaTM C18色谱柱(250 mm×4.6 mm, 5 μm)分离,所用流动相为乙腈(A)和0.1%甲酸水溶液(B),梯度洗脱,流速为0.8 mL/min;用紫外检测器检测新芒果苷与芒果苷,检测温度为室温,检测波长为265 nm。用蒸发光散射检测器检测知母皂苷BIII、知母皂苷I和知母皂苷AIII,漂移管温度为50 ℃,气体压力为179.1 kPa(26 psi)。知母经炮制后,5种化合物含量均发生了不同程度的改变,表明炮制方法的不同对知母化学成分的含量影响较大。该方法对进一步研究炮制方法对知母的药效学影响提供了一定的参考依据。

关键词: 高效液相色谱;新芒果苷;芒果苷;知母皂苷BIII;知母皂苷I;知母皂苷AIII;知母;炮制

文章编号: 1000-8713(2012)12-1271-05

 

Effects of different processing methods on five main chemical constituents of Anemarrhena asphodeloides Bge. studied by high performance liquid chromatography

ZHAO Lulu1, LIU Feifei1, PENG Ying1,2*, KANG Tingguo2

(1. School of Traditional Chinese Materia Medica, Shenyang Pharmaceutical University, Shenyang 110016, China; 2. Liaoning University of Traditional Chinese Medicine, Shenyang 110032, China)

Abstract: A high performance liquid chromatographic (HPLC) method has been developed for the simultaneous determination of neomangiferin, mangiferin, timosaponin BIII, anemarrhenasaponin I and timosaponin AIII in the products of Anemarrhena asphodeloides Bge. processed by different methods. By comparing and analyzing the variation of the contents of the five components, the effects of processing on chemical constituents of Anemarrhena asphodeloides Bge. were explored, which provided evidences for the relevance between processing and the property changes of Anemarrhena asphodeloides Bge. The chromatographic separation was performed on an AlltimaTM C18 column (250 mm×4.6 mm, 5 μm) with a gradient elution of acetonitrile (A) and 0.1% formic acid (B) (0~10 min, 5%A~20%A; 10~15 min, 20%A~25%A; 15~30 min, 25%A~80%A; 30~35 min, 80%A~100%A) at a flow rate of 0.8 mL/min. Neomangiferin and mangiferin were detected by an ultraviolet detector at 265 nm and room temperature. Timosaponin BIII, anemarrhenasaponin I and timosaponin AIII were detected by an evaporative light scattering detector with the drift temperature at 50 ℃ and gas pressure at 179.1 kPa (26 psi). To some extent, the contents of the major components varied in different processed products of Anemarrhena asphodeloides Bge. The results indicated that different processing methods caused significant differences in the contents of the major components of Anemarrhena asphodeloides Bge. It is of great use for further researching the relevance of the processing methods to pharmacodynamics of Anemarrhena asphodeloides Bge.

Key words: high performance liquid chromatography (HPLC); neomangiferin; mangiferin; timosaponin BIII; anemarrhenasaponinI; timosaponin AIII; Anemarrhena asphodeloides Bge.; processing

 

1276-1281

DOI: 10.3724/SP.J.1123.2012.09044

*通讯联系人: 徐远金,博士,教授,研究方向为色谱-质谱分析. Tel: (0771)3237743, E-mail: yjxu@gxu.edu.cn.

基金项目: 国家自然科学基金项目(20865001)和广西自然科学基金项目(桂科自0832034).

收稿日期: 2012-09-29

 

月桂酰基苹果酸酯胶束电动色谱-质谱法同时测定牛黄上清片中5种生物碱

胡梦迪1,2, 苏迪1,2, 范晓苏1,2, 于建华2, 徐远金1,2*

(1. 亚热带农业生物资源保护与利用国家重点实验室, 广西 南宁 530004; 2. 广西大学化学化工学院, 广西 南宁 530004)

摘要: 建立了基于月桂酰基苹果酸酯的胶束电动色谱-质谱法同时分离测定牛黄上清片中黄连碱、小檗碱、药根碱、黄柏碱以及川芎嗪5种有效成分含量的新方法。以7.5 mmol/L月桂酰基苹果酸酯-15 mmol/L氨水-50 mmol/L醋酸铵(含12.5%的乙腈,pH=7.0)为电泳介质,未涂层弹性石英毛细管(88 cm×50 μm)为分离通道,50%异丙醇水溶液(含3 mmol/L乙酸)为鞘液,在25 kV的运行电压下,各组分可以在18 min内得到基线分离。各组分的浓度与其峰面积呈现良好的线性关系,迁移时间和峰面积的相对标准偏差均小于5%,样品中5种生物碱成分的样品加标回收率在96.0%-105%之间。该法简便、快速、准确、重现性好,可用于牛黄上清片中这5种有效成分含量的同时测定。

关键词: 胶束电动色谱;电喷雾离子化质谱法;月桂酰基苹果酸酯;生物碱;牛黄上清片

文章编号: 1000-8713(2012)12-1276-06

 

Simultaneous determination of five alkaloids in Niuhuang Shangqing Tablets by micellar electrokinetic chromatography-mass spectrometry using laurel acyl malic acid ester

HU Mengdi1,2, SU Di1,2, FAN Xiaosu1,2, YU Jianhua2, XU Yuanjin1,2*

(1. State Key Laboratory of Conservation and Utilization of Subtropical Agro-bioresources, Nanning 530004, China, 2. School of Chemistry and Chemical Engineering, Guangxi University, Nanning 530004, China)

Abstract: A micellar electrokinetic chromatography-mass spectrometric method based on laurel acyl malic acid ester (LMAE) for the separation and determination of coptisine, berberine, jatrorrhizine, phellodendrine and ligustrazine in Niuhuang Shangqing Tablets was established. The baseline separation of the five compounds was attained within 18 min by an uncoated capillary (88 cm×50 μm) on the operating voltage of 25 kV using 7.5 mmol/L LMAE-15 mmol/L ammonia-50 mmol/L ammonium acetate mixture (pH=7.0) containing 12.5% (v/v) acetonitrile as the electrophoretic medium and 50% 2-propanol aqueous solution (containing 3 mmol/L acetic acid) as the sheath liquid. The peak area of each component to its concentration showed a good linear relationship. The relative standard deviations of migration times and peak areas of the five components were less than 5% and the recoveries were between 96.0% and 105%. The developed method is simple, rapid, accurate and is suitable for the routine analysis of the five alkaloid components in Niuhuang Shangqing Tablets.

Key words: micellar electrokinetic chromatography (MEKC); electrospray ionization-mass spectrometry (ESI-MS); laurel acyl malic acid ester; alkaloids; Niuhuang Shangqing Tablets

 

1282-1286

DOI: 10.3724/SP.J.1123.2012.07037

*通讯联系人: 施超欧,高级工程师,研究方向为离子色谱、液相色谱的开发与应用. E-mail: HPLC@ecust.edu.cn.

收稿日期: 2012-07-19

 

并联式双三元高效液相色谱系统快速检测土壤中6种蒽醌类化合物

马浩, 贺伟, 杨柳, 尹雪梅, 王文佳, 施超欧*

(华东理工大学分析测试中心, 上海 200237)

摘要: 建立了用于住宅建设污染土壤中1,8-二硝基蒽醌、1,5-二硝基蒽醌、1-氨基蒽醌、蒽醌、萘、1,4,5,8-四氯蒽醌等6种蒽醌类化合物含量的高效液相色谱分析方法。利用Ultimate双三元液相色谱仪的特点,设计了一套并联式双系统,采用2根相同的色谱柱(Dikma Diamonsil C18)交叉分析,节省了41.46%的分析时间。以50 mL N,N-二甲基甲酰胺-1,4-二氧六环-甲醇(5:20:25, v/v/v)为萃取剂,采用超声波辅助方法提取样品中的6种目标物。6种目标物的平均加标回收率为82.7%-101%,相对标准偏差为1.8%-3.2%,检出限(以信噪比为3计)为0.007-0.054 mg/kg,可满足北京地方标准DB11/T 811-2011的限量要求。该方法简便、准确,并能节省检测时间,有良好的重现性,可用于土壤中蒽醌类化合物的检测。

关键词: 高效液相色谱;并联式双梯度;蒽醌类化合物;土壤

文章编号: 1000-8713(2012)12-1282-05

 

Determination of six anthraquinone compounds in soil by parallel type dual gradient high performance liquid chromatography

MA Hao, HE Wei, YANG Liu, YIN Xuemei, WANG Wenjia, SHI Chaoou*

(Analysis and Research Center, East China University of Science and Technology, Shanghai 200237, China)

Abstract: A high performance liquid chromatography (HPLC) was established for the determination of six anthraquinone compounds, 1,8-dinitroanthraquinone, 1,5-dinitroanthraquinone, 1-aminoanthraquinone, anthraquinone, naphthalene, 1,4,5,8-tetrachlorodibenzo anthraquinone, in polluted soil of residential construction. In this method, by using an Ultimate dual gradient liquid chromatograph (DGLC), designing a set of parallel dual system and accepting two same Dikma Diamonsil C18 columns (150 mm×4.6 mm, 5 μm) to cross-analysis, 41.46% of the analysis time can be saved. By using assisted ultrasonication to the extraction of the six substances in the samples with 50 mL N,N-dimethyl-formamide/1,4-dioxane/methanol (5/20/25, v/v/v), the average recoveries of the six analytes spiked in nine blank soil samples were 82.7%~101% with the relative standard deviations (RSDs) of 1.8%~3.2% and the limits of detection were 0.007~0.054 mg/kg, which can reach the limited requirement of the local standard in Beijing of DB11/T 811-2011. With the advantages of accessibility, high sensitivity and good reproducibility, this method can be used in the determination of anthraquinone compounds in soil.

Key words: high performance liquid chromatography (HPLC); parallel type dual gradient; anthraquinone compounds; soil

 

1287-1291

DOI: 10.3724/SP.J.1123.2012.04042

*通讯联系人: 吕春华,博士,高级工程师,主要研究方向为理化检验. E-mail: lvch@ziq.gov.cn.

基金项目: 国家质量监督检验检疫总局课题.

收稿日期: 2012-07-22

 

柱前衍生-萃取阻断反应-高效液相色谱法测定化妆品中游离甲醛

吕春华1*, 黄超群1, 陈梅2, 谢文1, 陈笑梅1

(1. 浙江出入境检验检疫局, 浙江 杭州 310016; 2. 浙江工业大学化学工程与材料学院, 浙江 杭州 310014)

摘要: 建立了柱前衍生化-萃取阻断反应-高效液相色谱(HPLC)测定化妆品中甲醛的方法。化妆品中甲醛检测的难点是: 甲醛缓释剂类防腐剂在衍生过程中释放甲醛,影响游离甲醛的准确测定。以2,4-二硝基苯肼(DNPH)乙腈溶液-磷酸盐缓冲液(pH 2)(1:1, v/v)为提取溶液,于室温下快速衍生2 min后,立即加入二氯甲烷萃取,阻断衍生反应,经乙腈稀释后进行HPLC测定。以Agilent C18柱(250 mm×4.6 mm, 5 μm)为分离柱,乙腈-水(60:40, v/v)为流动相,流速为1.0 mL/min,于355 nm波长下检测。在洗发水、乳液、膏霜、洗手液、牙膏、指甲油、粉饼中分别添加50、100、500、1000 μg/g 4个浓度水平的甲醛,其回收率为81%-106%,相对标准偏差(n=6)<5.0%。方法的定量限(以信噪比(S/N)>10计)为50 μg/g。该方法快速、简便、重现性好,且可以有效避免甲醛缓释剂类防腐剂分解释放甲醛,适用于化妆品中游离甲醛的测定。

关键词: 高效液相色谱法;柱前衍生;甲醛缓释剂;游离甲醛;化妆品

文章编号: 1000-8713(2012)12-1287-05

 

Determination of free formaldehyde in cosmetics by pre-column derivatization, extraction inhibition and high performance liquid chromatography

L Chunhua1*, HUANG Chaoqun1, CHEN Mei2, XIE Wen1, CHEN Xiaomei1

(1. Zhejiang Entry-Exit Inspection and Quarantine Bureau, Hangzhou 310016, China; 2. College of Chemical Engineering and Materials Science, Zhejiang University of Technology, Hangzhou 310014, China)

Abstract: Pre-column derivatization and inhibition by solvent extraction were applied to determine free formaldehyde in cosmetics by high performance liquid chromatography (HPLC). Due to the rapid decomposition of formaldehyde donors in the derivatization, it is hard to detect the amount of the free formaldehyde in cosmetics. The formaldehyde directly reacted with 2,4-dinitrophenylhydrazine in acetonitrile-phosphate buffer (pH 2) (1:1, v/v) solution for 2 min, then dichloromethane extraction was used to induce the decomposition of formaldehyde donors. The extract was diluted with acetonitrile and then determined by HPLC. The formaldehyde derivative was separated on an Agilent C18 column (250 mm×4.6 mm, 5 μm) at 30 ℃ with acetonitrile-water (60:40, v/v) as mobile phase at a flow rate of 1.0 mL/min, and detected at the wavelength of 355 nm. The recoveries were from 81% to 106% at the spiked levels of 50, 100, 500, 1000 μg/g of formaldehyde in shampoo, milk, cream, hand cleaner, toothpaste, nail polish, powder separately, and the relative standard deviations (n=6) were less than 5.0%. The limit of quantification of the formaldehyde in cosmetics was 50 μg/g. The method has been applied to the determination of free formaldehyde in real samples and the results showed that the release by formaldehyde donors was inhibited. The method has the advantages of simple operation, good accuracy and meets the requirement of determination of free formaldehyde in cosmetics.

Key words: high performance liquid chromatography (HPLC); pre-column derivatization; formaldehyde donors; free formaldehyde; cosmetics

 

1292-1294

DOI: 10.3724/SP.J.1123.2012.08044

*通讯联系人: 牛长群,正高级工程师,主要从事新药研究开发工作. Tel: (0311)86993040, E-mail: niuchangqun@126.com.

收稿日期: 2012-08-24

 

反相离子对色谱法测定脱氧精胍菌素药物中的主成分

程晓昆, 王娅莉, 张惠敏, 牛长群*

(华北制药集团新药研究开发有限责任公司, 河北 石家庄 050015)

摘要: 建立了反相离子对色谱法分离测定脱氧精胍菌素药物中主成分的方法。分别考察了色谱柱类型、离子对试剂种类及浓度、缓冲盐浓度和流动相pH值等参数对实验结果的影响。确定了分离脱氧精胍菌素的最佳条件: C18色谱柱(250 mm×4.6 mm, 5 μm);以5 mmol/L磷酸氢二钾水溶液(含5 mmol/L戊烷磺酸钠,pH 3.6±0.3)-乙腈(90:10, v/v)为流动相,流速为1.0 mL/min;检测波长为210 nm;柱温为30 ℃;进样量为20 μL。该方法实现了对脱氧精胍菌素的良好分离,且线性关系良好,检出限可达0.5 mg/L。

关键词: 反相高效液相色谱法;离子对试剂;脱氧精胍菌素;药物

文章编号: 1000-8713(2012)12-1292-03

 

Determination of a major constituent in deoxyspergualin drug by reversed-phase ion-pair chromatography

CHENG Xiaokun, WANG Yali, ZHANG Huimin, NIU Changqun*

(North China Pharmaceutical Group New Drug Research and Development Co., Ltd, Shijiazhuang 050015, China)

Abstract: A method was established for the determination of deoxyspergualin using reversed-phase ion-pair chromatography (RP-IPC). Several parameters, such as the chromatographic column, the types and concentration of ion-pair reagents, the concentration of the buffer and the pH value of the mobile phase were evaluated. The optimal separation conditions were as follows: C18 column (250 mm×4.6 mm, 5 μm); mobile phase, 5 mmol/L di-potassium hydrogen phosphate (containing 5 mmol/L 1-pentanesulfonic acid sodium, pH 3.6±0.3)-acetonitrile (90:10, v/v); flow rate, 1.0 mL/min; detection wavelength, 210 nm; column temperature, 30 ℃; injection volume, 20 μL. Under the optimaized experimental conditions, good linear relationships was obtained and the limit of detection for deoxyspergualin was 0.5mg/L.

Key words: reversed-phase ion-pair chromatography (RP-IPC); ion-pair reagents; deoxyspergualin (DSG); drug

 

1295-1300

DOI: 10.3724/SP.J.1123.2012.09007

*通讯联系人: 曹丽伟,博士,副教授,研究方向为生物分子探针. E-mail: lwcao@126.com.

基金项目: 国家自然科学基金青年项目(21205049).

收稿日期: 2012-09-05

 

毛细管电泳-激光诱导荧光法测定草甘膦、草胺膦及氨甲基膦酸

曹丽伟*, 梁丝柳, 谭小芳, 孟建新

(暨南大学生命科学技术学院化学系, 广东 广州 510632)

摘要: 建立了一种快速、有效的毛细管电泳分离-激光诱导荧光检测有机磷除草剂草甘膦、草胺膦和草甘膦的代谢物氨甲基膦酸的方法。将荧光衍生试剂5-(4, 6-二氯三嗪基)氨基荧光素(DTAF)成功用于衍生上述3种化合物。最佳衍生条件: DTAF的浓度为1.0 μmol/L,以50 mmol/L硼酸(pH 9.5)作为缓冲溶液,在30 ℃下反应40 min。以pH 9.5的30 mmol/L硼酸缓冲溶液(含15 mmol/L Brij-35)作为电泳背景电解质,3种衍生物得到基线分离。在优化的条件下,草甘膦、草胺膦、氨甲基膦酸的检出限分别为3.21、6.14和1.99 ng/kg。将该方法应用于环境水样和土壤中除草剂及代谢物的测定,回收率为91.3%-106.0%。该方法准确、灵敏,可满足环境样品中有机磷农药及其代谢物残留的检测要求。

关键词: 毛细管电泳;激光诱导荧光检测;衍生;除草剂;土壤;水

文章编号: 1000-8713(2012)12-1295-06

 

Capillary electrophoresis analysis for glyphosate, glufosinate and aminomethylphosphonic acid with laser-induced fluorescence detection

CAO Liwei*, LIANG Siliu, TAN Xiaofang, MENG Jianxin

(Department of Chemistry, College of Life Science and Technology, Jinan University, Guangzhou 510632, China)

Abstract: A sensitive analytical method was developed for the simultaneous determination of glyphosate, glufosinate and aminomethylphosphonic acid by capillary electrophoresis with laser-induced fluorescence detection (CE-LIF). 5-(4,6-Dichlorotriazinyl) amino fluorescein (DTAF) was successfully applied to label the herbicides. The optimal derivatization reaction was carried out in boric acid buffer of pH 9.5 at 30 ℃ for 40 min. The baseline separation of the three derivatives could be accomplished using 30 mmol/L boric acid, 15 mmol/L Brij-35 (pH 9.5) as the running buffer. The detection limits (S/N=3) for the glyphosate, glufosinate and aminomethylphosphonic acid were 3.21, 6.14, 1.99 ng/kg, respectively. Finally, the method was successfully applied to the analysis of environmental samples, and the three compounds were measured without any interference from real samples. The recoveries of the compounds in these samples were 91.3%~106.0%. The method has the advantages of easiness and sensitivity, and can meet the requirement of the determination of the herbicide and metabolite residues in the environmental samples.

Key words: capillary electrophoresis (CE); laser-induced fluorescence detection (LIF); derivatization; herbicides; soil; water

 

 


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