QuEChERS法提取-气相色谱-串联质谱法测定生态纺织品中31种农药残留
QuEChERS-GC-MS/MS Determination of 31 Pesticide Residues in Ecological Textile
摘 要
采用QuEChERS法提取-气相色谱-串联质谱法同时测定生态纺织品中31种农药残留。样品粉碎后用乙腈萃取,提取液经无水硫酸镁和氯化钠除水后,用乙二胺-N-丙基硅烷和C18吸附剂净化,离心后过膜。待测物在Thermo TR-RESTICIDE石英毛细管色谱柱上分离,采用电子轰击离子源和选择反应监测模式进行质谱测定。31种农药的线性范围均为0.01~1.00 mg·L-1,检出限(3S/N)在0.005~0.007 mg·kg-1之间。加标回收率在80.3%~99.9%之间,测定值的相对标准偏差(n=6)小于7.0%。
QuEChERS方法
农药残留
生态纺织品
GC-MS/MS
QuEChERS
Pesticide residues
Ecological textiles
Abstract
QuEChERS-GC-MS/MS was applied to the determination of 31 pesticide residues in ecological textiles. The sample was splintered and then extracted with acetonitrile. The extract was dehydrated with anhydrous magnesium sulfate and sodium chloride, purified with ethylenediamine-N-propylsilane and C18 adsorbent, then centrifuged and filtrated for GC-MS/MS analysis. The analytes were separated on a Thermo TR-RESTICIDE capillary chromatographic column. EI and SRM were adopted in MS. The linearity ranges of the 31 pesticides were found 0.01-1.00 mg·L-1 with detection limits (3S/N) in the range of 0.005-0.007 mg·kg-1. Recovery rates obtained by standard addition method were in the range of 80.3%-99.9%, and RSDs (n=6) were less than 7.0%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201510008
所属栏目 工作简报
基金项目 国家质检总局公益性行业科研课题(201310056)
收稿日期 2014/9/15
修改稿日期
网络出版日期
作者单位点击查看
联系人作者冯伟(gshteng@163.com)
备注冯伟(1988-),男,江西九江人,硕士研究生,主要研究方向为有机分析。
引用该论文: FENG Wei,ZHANG Dai-hui,ZHANG Xun,YANG Lu,ZHAO Yun-hui,TENG Guo-sheng. QuEChERS-GC-MS/MS Determination of 31 Pesticide Residues in Ecological Textile[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(10): 1386～1392
冯伟,张代辉,张勋,杨璐,赵韫慧,滕国生. QuEChERS法提取-气相色谱-串联质谱法测定生态纺织品中31种农药残留[J]. 理化检验－化学分册, 2015, 51(10): 1386～1392
被引情况:
【1】陈兆波,顾虎,秦鑫, "单滴微萃取-气相色谱-质谱法测定纺织品中8种抗菌剂",理化检验－化学分册 52, 1375-1379(2016)
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参考文献
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【20】PLCIDO A, PAGA P, LOPES D, et al. Determination of methiocarb and its degradation products, methiocarb sulfoxide and methiocarb sulfone, in bananas using QuEChERS extraction［J］. Journal of Agricultural and Food Chemistry, 2013,61(2):325-331.
【21】宋莹,张耀海,黄霞,等.气相色谱-串联质谱法快速检测水果中的多效唑残留［J］.分析化学, 2011,39(8):1270-1273.
【22】张雪莲,张耀海,焦必宁.气相色谱-串联质谱法结合QuEChERS方法快速检测柑橘中52种农药多残留［J］.食品科学, 2013,34(6):152-155.
【23】陈晓水,边照阳,杨飞,等.对比3种不同的QuEChERS前处理方式在气相色谱-串联质谱检测分析烟草中上百种农药残留中的应用［J］.色谱, 2013,31(11):1116-1128.
【2】王国庆,张东飞,王素方,等.气相色谱-质谱法测定水果中杀菌剂残留量［J］.理化检验-化学分册, 2010,46(2):197-199.
【3】CAI Jin-an, ZHU Fang, RUAN Wen-hong, et al. Determination of organochlorine pesticides in textile using solid-phase microextraction with gas chromatography-mass spectrometry［J］. Microchemical Journal, 2013,110(9):280-284.
【4】KE Yuan-yuan, ZHU Fang, ZENG Feng, et al. Preparation of graphene-coated solid-phase microextraction fiber and its application on organochlorine pesticides determination［J］. Journal of Chromatography, 2013,1300(7):187-192.
【5】张翔,廖青,张焱,等.高效液相色谱法同时检测棉织品中的9种有机氯农药残留［J］.色谱, 2007,25(3):380-383.
【6】谢洪学,何丽君,伍艳,等.基于离子液体的液相微萃取-高效液相色谱法测定水中有机磷农药［J］.分析化学, 2007,35(2):187-190.
【7】WONG J W, ZHANG Kai, TECH K, et al. Multiresidue pesticide analysis of ginseng powders using acetonitrile-or acetone-based extraction, solid-phase extraction cleanup, and gas chromatography-mass spectrometry/selective ion monitoring (GC-MS/SIM) or-tandem mass spectrometry (GC-MS/MS)［J］. Journal of Agricultural and Food Chemistry, 2010,58(10):5884-5896.
【8】FINTSCHENKO Y, KRYNITSKY A J, WONG J W. Emerging pesticide residue issuesand analytical approaches［J］. Journal of Agricultural and Food Chemistry, 2010,58(10):5859-5861.
【9】MASTOVSKA K, DORWEILER K J, LEHOTAY S J, et al. Pesticide multiresidue analysis in cereal grains using modified QuEChERS method combined with automated direct sample introduction GC-TOFMS an UPLC-MS/MS techniques［J］. Journal of Agricultural and Food Chemistry, 2010,58(10):5959-5972.
【10】MATOVSK K, LEHOTAY S J, ANASTASSIADES M. Combination of analyte protectants to overcome matrix effects in routine GC analysis of pesticide residues in food matrixes［J］. Analytical Chemistry, 2005,77(24):8129-8137.
【11】PREZ I S, CULZONI M J, SIANO G G, et al. Detection of unintended stress effects based on a metabonomic study in tomato fruits after treatment with carbofuran pesticide. Capabilities of MCR-ALS applied to LC-MS three-way data arrays［J］. Analytical Chemistry, 2009,81(20):8335-8346.
【12】柳彩云,马微,陈伟,等.气相色谱-质谱法测定纺织品中22种农药残留［J］.理化检验-化学分册, 2012,48(11):1303-1306.
【13】徐宜宏,姜玲玲,杨潇,等.纺织品中农药残留检测技术的研究进展［J］.毛纺科技, 2014,42(3):61-64.
【14】王连珠,周昱,陈泳,等.样品前处理-液相色谱-串联质谱法测定蔬菜中66种有机磷农药残留量方法评估［J］.色谱, 2012,30(2):146-153.
【15】马智玲,赵文,李凌云,等.气相色谱-三重四极杆串联质谱法快速测定蔬菜水果中129种农药的残留量［J］.色谱, 2013,31(3):228-239.
【16】XIA Kang, ATKINS J, FOSTER C, et al. Analysis of cyromazine in poultry feed using the QuEChERS method coupled with LC-MS/MS［J］. Journal of Agricultural and Food Chemistry, 2010,58(10):5945-5949.
【17】张志勇,龚勇,单炜力,等.QuEChERS-高效液相色谱-串联质谱法测定黄瓜和土壤中甲基硫菌灵和多菌灵［J］.色谱, 2012,30(1):91-94.
【18】梅梅,杜振霞,陈芸.QuEChERS-超高效液相色谱串联质谱法同时测定土壤中5种常用除草剂［J］.分析化学, 2011,39(11):1659-1664.
【19】CALDAS S, BOLZAN C, CERQUEIRA M, et al. Primel evaluation of a modified QuEChERS extraction of multiple classes of pesticides from a rice paddy soil by LC-APCI-MS/MS［J］. Journal of Agricultural and Food Chemistry, 2011,59(22):11918-11926.
【20】PLCIDO A, PAGA P, LOPES D, et al. Determination of methiocarb and its degradation products, methiocarb sulfoxide and methiocarb sulfone, in bananas using QuEChERS extraction［J］. Journal of Agricultural and Food Chemistry, 2013,61(2):325-331.
【21】宋莹,张耀海,黄霞,等.气相色谱-串联质谱法快速检测水果中的多效唑残留［J］.分析化学, 2011,39(8):1270-1273.
【22】张雪莲,张耀海,焦必宁.气相色谱-串联质谱法结合QuEChERS方法快速检测柑橘中52种农药多残留［J］.食品科学, 2013,34(6):152-155.
【23】陈晓水,边照阳,杨飞,等.对比3种不同的QuEChERS前处理方式在气相色谱-串联质谱检测分析烟草中上百种农药残留中的应用［J］.色谱, 2013,31(11):1116-1128.
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