气相色谱-串联质谱法测定鲜香菇中25种有机磷类农药残留
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摘要
建立了气相色谱-串联质谱测定香菇中25种有机磷农药残留的检测方法。样品用氯化钠、乙腈提取,C18分散固相萃取净化。采用EI源电离多反应监测(MRM)模式进行检测,基质标准溶液校正,外标法定性、定量。分别讨论了氯化钠加入先后顺序对提取效果的影响和C18的用量对净化效果的影响。结果表明,25种化合物色谱峰分离度高,在各自的线性范围内线性关系良好(r2>0.99),在3个添加水平下的平均回收率为70.7%～116.6%,相对标准偏差(RSD)为4.4%～14.0%,方法的定量限为0.002～0.010 mg·kg-1。该方法简单、快速,能保证批量样品连续检测的稳定性,适用于香菇样品中多种有机磷类农药残留的同时检测。
A method was developed for the determinations of 25 organophosphorus pesticides in shiitake using gas chromatography-tandem mass spectrometry technique. The sample ware extracted by sodium chloride and acetonitrile.Then the extracts were purified by dispersive solid phase extraction with C18. The solvent extracts were analyzed by GC-MS/MS in the EI ion mode and multiple reaction monitoring(MRM)mode. The matrix standard solutions were used for calibration. External standard was used as the qualitative and quantitative method. The extraction effect of NaCl addition sequence and the purification effect of C18 dosage were discussed respectively. The results showed that 25 pesticides had good linearity within their respective linear range(r2> 0.99),the average recoveries at three spiked levels ranged from 70.7 % to 116.6 % with the relative standard deviations(RSDs)from 4.4 %-14.0 %. The limits of quantification of this method were in the range of 0.002-0.010 mg · kg-1. This method is simple,quick and has a good stability of the continuous batch analysis. It is suitable for determination of multiple organophosphorus pesticides in shiitake simultaneously.
A method was developed for the determinations of 25 organophosphorus pesticides in shiitake using gas chromatography-tandem mass spectrometry technique. The sample ware extracted by sodium chloride and acetonitrile.Then the extracts were purified by dispersive solid phase extraction with C18. The solvent extracts were analyzed by GC-MS/MS in the EI ion mode and multiple reaction monitoring(MRM)mode. The matrix standard solutions were used for calibration. External standard was used as the qualitative and quantitative method. The extraction effect of NaCl addition sequence and the purification effect of C18 dosage were discussed respectively. The results showed that 25 pesticides had good linearity within their respective linear range(r2> 0.99),the average recoveries at three spiked levels ranged from 70.7 % to 116.6 % with the relative standard deviations(RSDs)from 4.4 %-14.0 %. The limits of quantification of this method were in the range of 0.002-0.010 mg · kg-1. This method is simple,quick and has a good stability of the continuous batch analysis. It is suitable for determination of multiple organophosphorus pesticides in shiitake simultaneously.
引文
[1]王丽娜,冯敏铃,李盛安,等.气相色谱法测定干香菇中9种有机磷农药的残留[J].广东化工,2016,43(19):174-175.
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[11]王连珠,周昱,陈泳,等.QuEChERS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.
[12]徐娟,陈捷,叶弘毅,等.QuEChERS提取与高效液相色谱-电喷雾电离串联质谱联用法检测茶叶中的19种农药残留[J].分析测试学报,2011,30(9):990-995.
[13]徐娟,陈捷,王岚,等.QuEChERS提取与超高效液相色谱-电喷雾电离串联质谱联用法检测果蔬中的230种农药残留[J].分析测试学报,2013,32(3):293-301.
[14] STEVEN J L,KYUNG A S,HYEYOUNG K,et al.Comparison of QuEChERS sample preparation methods for the analysis of pesticide residues in fruits and vegetables[J].Journal of Chromatography A,2010,1217(16):2548-2560.
[15] HE Z Y,WANG Y H,WANG L,et al.Determination of 255pesticides in edible vegetable oils using QuEChERS and gas chromatography tandem mass spectrometry[J].Analytical and Bioanalytical Chemistry,2017,409(4):1017-1030.
[16]黎小鹏,李拥军,刘红梅,等.QuEChERS前处理-高效液相色谱仪检测多种蔬菜水果中10种氨基甲酸酯农药残留[J].现代农业科技,2014(13):138-140.
[17]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]白冰,董茂锋,邢增涛,等.气相色谱-质谱法检测双孢蘑菇和香菇中的67种农药残留[J].食用菌学报,2011,18(1):63-69.
[3]董娇,邰丽梅.国内外食用菌农药残留限量标准比较分析[J].中国食用菌,2017,36(5):1-5.
[4]单美娜,徐晓枫,蒲云霞,等.固相萃取-气相色谱法测定食用菌中有机磷农药残留[J].中国卫生检验杂志,2015,25(2):176-178.
[5] BI S Y,ZHU Z Q,CHI W H,et al.Determination of eight organophosphorus pesticide residues in pepper by QuEChERS-Gas chronmatography[J].Agricultural Biotechnology,2018,7(1):123-125.
[6]韩梅,侯雪.气相色谱串联质谱法测定香菇中几种氨基甲酸酯农药残留量[J].中国测试,2013,39(1):52-55.
[7]吴延灿,商鲁宁,戚传勇,等.QuEChERS-气相色谱-串联质谱法测定香菇中29种农药残留[J].食品安全质量检测学报,2017,8(9):3594-3600.
[8]王会锋,冯书惠,贾斌.香菇中40种农药残留量的气相色谱法测定[J].食品科学,2010,31(20):335-341.
[9]张爱芝,王全林,曹丽丽,等.QuEChERS-超高效液相色谱-串联质谱法测定蔬菜中250种农药残留[J].色谱,2016,34(2):158-164.
[10]李春艳.QuEChERS法-色质联用技术在农药残留检测应用中的研究[D].西安:西安理工大学,2010.
[11]王连珠,周昱,陈泳,等.QuEChERS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.
[12]徐娟,陈捷,叶弘毅,等.QuEChERS提取与高效液相色谱-电喷雾电离串联质谱联用法检测茶叶中的19种农药残留[J].分析测试学报,2011,30(9):990-995.
[13]徐娟,陈捷,王岚,等.QuEChERS提取与超高效液相色谱-电喷雾电离串联质谱联用法检测果蔬中的230种农药残留[J].分析测试学报,2013,32(3):293-301.
[14] STEVEN J L,KYUNG A S,HYEYOUNG K,et al.Comparison of QuEChERS sample preparation methods for the analysis of pesticide residues in fruits and vegetables[J].Journal of Chromatography A,2010,1217(16):2548-2560.
[15] HE Z Y,WANG Y H,WANG L,et al.Determination of 255pesticides in edible vegetable oils using QuEChERS and gas chromatography tandem mass spectrometry[J].Analytical and Bioanalytical Chemistry,2017,409(4):1017-1030.
[16]黎小鹏,李拥军,刘红梅,等.QuEChERS前处理-高效液相色谱仪检测多种蔬菜水果中10种氨基甲酸酯农药残留[J].现代农业科技,2014(13):138-140.
[17]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.