UHPLC-MS/MS Determination of 7 Carbamate Pesticides and Metabolites Residues in Artemisia Selengensis
摘 要
采用超高效液相色谱串联质谱法(UHPLC-MS/MS)测定芦蒿中7种氨基甲酸酯类农药及其代谢物残留。取芦蒿样品5.00 g,用乙腈10 mL超声提取5 min,提取液用6.0 g硫酸镁和1.5 g乙酸钠脱水后,经QuECHERS固相萃取柱净化。净化液用(A) 10 mmol·L-1甲酸铵溶液和(B) 10 mmol·L-1甲酸铵-甲醇溶液的体积比为9∶1的混合液稀释至0.8 mL后进行色谱分离,以Kinetex C18 100A色谱柱为固定相,以不同体积比的上述两种溶液(A和B)的混合液为流动相进行梯度洗脱。质谱分析中采用电喷雾正离子源和多反应监测模式。7种化合物的线性范围均在0.50~20.0 μg·L-1之间;检出限(3S/N)为0.17~0.55 μg·kg-1。加标回收率为67.4%~103%;测定值的相对标准偏差(n=6)在1.1%~8.5%之间。
Abstract
UHPLC-MS/MS was applied to the determination of 7 kinds of carbamate pesticides and metabolites residues in artemisia selengensis. Sample of artemisia selengensis (5.00 g) was extracted ultrasonically with 10 mL of acetonitrile, and the extract was dehydrated by adding 6.0 g of MgSO4 and 1.5 g of NaOAc. The extract was then purified by passing through QuECHERS SPE column. The purified extract was diluted to 0.8 mL with a mixture of (A) 10 mmol·L-1 ammonium formate solution and (B) 10 mmol·L-1 ammonium formate methanol solution mixed in the ratio of 9∶1, and the diluted solution was then separated by UHPLC using Kinetex C18 100A column as stationary phase and mixtures of ammonium formate solution of (A) and (B) mentioned above in various ratios as mobile phase in gradient elution. In MS/MS, ESI+ and MRM were adopted. Linearity ranges for the 7 compounds were obtained to be same between 0.50-20.0 μg·L-1, and values of detection limits (3S/N) found were in the range of 0.17-0.55 μg·kg-1. Recovery was tested by standard addition method, giving results of recovery in the range of 67.4%-103%, and of RSDs (n=6) ranged from 1.1% to 8.5%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201611005
所属栏目 工作简报
基金项目 南京市科技发展资金资助(YKK14166;QRX11128)
收稿日期 2016/2/6
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备注刘祥萍(1974-),女,山东郯城人,副主任技师,博士,主要从事食品污染物和生活饮水中有害物质分析。
引用该论文: LIU Xiang-ping,SUN Wen-fang,HUANG Wei,LIN Jie. UHPLC-MS/MS Determination of 7 Carbamate Pesticides and Metabolites Residues in Artemisia Selengensis[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2016, 52(11): 1262~1266
刘祥萍,孙文芳,黄薇,林洁. 超高效液相色谱-串联质谱法测定芦蒿中7种氨基甲酸酯类农药及其代谢物残留量[J]. 理化检验-化学分册, 2016, 52(11): 1262~1266
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参考文献
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【2】左海根,占春瑞.生姜中涕灭威及涕灭威砜的GC分析方法研究[J].分析试验室, 2008,27(增1):311-314.
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【8】田宏哲,赵瑛博,周艳明.高效液相色谱-质谱法测定牛奶中6种氨基甲酸酯农药残留[J].食品科学, 2011,32(2):187-190.
【9】王静,刘铮铮,钟光剑.超高效液相色谱-串联质谱法分析土壤及沉积物中氨基甲酸酯农药[J].中国环境监测, 2013,29(4):103-106.
【10】徐远金,李永库.中药材中氨基甲酸酯类农药的高效液相色谱-质谱分析[J].理化检验-化学分册, 2006,42(11):877-880.
【11】于峰.农药克百威和丁硫克百威的质谱分析[J].质谱学报, 2000,21(3/4):63-64.
【12】SOLER C, HAMILTON B, FUREY A, et al. Optimization of LC-MS/MS using triple quadrupole mass analyzer for the simultaneous analysis of carbosulfan and its main metabolites in oranges[J]. Anal Chim Acta, 2006,571(1):1-11.
【13】SHALLIKER R A, GUIOCHON G. Understanding the importance of the viscosity contrast between the sample solvent plug and the mobile phase and its potential consequence in two-dimensional high-performance liquid chromatography[J]. J Chromatogr A, 2009,1216(5):787-793.
【14】杨欣,李鹏,苗虹,等.凝胶渗透色谱-高效液相色谱-线性离子阱质谱法测定膳食样品中的氨基甲酸酯类农药残留[J].色谱, 2014,32(5):499-505.
【15】GB 2763-2014食品安全国家标准 食品中农药最大残留限量[S].
【2】左海根,占春瑞.生姜中涕灭威及涕灭威砜的GC分析方法研究[J].分析试验室, 2008,27(增1):311-314.
【3】郝宁.蔬菜、水果中16种有机磷和氨基甲酸酯农药残留检测方法研究[J].职业与健康, 2012,28(4):430-434.
【4】万益群,李申杰,鄢爱平.白术中有机磷及氨基甲酸酯类农药残留量的测定[J].分析科学学报, 2007,23(3):299-302.
【5】孙福江,李润岩,原现瑞,等.顶空固相微萃取-气质联用法检测苹果中氨基甲酸酯类农药残留[J].食品科学, 2010,31(10):223-227.
【6】丁涛,徐锦忠,沈崇钰,等.高效液相色谱-柱后衍生和质谱联用测定大米中氨基甲酸酯类农药残留量[J].分析试验室, 2007,26(9):77-80.
【7】周长朋,杨丽君,徐成钢,等.高效液相色谱-串联质谱法测定蔬菜中氨基甲酸类农药残留量[J].分析科学学报, 2011,27(4):487-490.
【8】田宏哲,赵瑛博,周艳明.高效液相色谱-质谱法测定牛奶中6种氨基甲酸酯农药残留[J].食品科学, 2011,32(2):187-190.
【9】王静,刘铮铮,钟光剑.超高效液相色谱-串联质谱法分析土壤及沉积物中氨基甲酸酯农药[J].中国环境监测, 2013,29(4):103-106.
【10】徐远金,李永库.中药材中氨基甲酸酯类农药的高效液相色谱-质谱分析[J].理化检验-化学分册, 2006,42(11):877-880.
【11】于峰.农药克百威和丁硫克百威的质谱分析[J].质谱学报, 2000,21(3/4):63-64.
【12】SOLER C, HAMILTON B, FUREY A, et al. Optimization of LC-MS/MS using triple quadrupole mass analyzer for the simultaneous analysis of carbosulfan and its main metabolites in oranges[J]. Anal Chim Acta, 2006,571(1):1-11.
【13】SHALLIKER R A, GUIOCHON G. Understanding the importance of the viscosity contrast between the sample solvent plug and the mobile phase and its potential consequence in two-dimensional high-performance liquid chromatography[J]. J Chromatogr A, 2009,1216(5):787-793.
【14】杨欣,李鹏,苗虹,等.凝胶渗透色谱-高效液相色谱-线性离子阱质谱法测定膳食样品中的氨基甲酸酯类农药残留[J].色谱, 2014,32(5):499-505.
【15】GB 2763-2014食品安全国家标准 食品中农药最大残留限量[S].
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