溶剂吸收气相色谱-质谱法测定蔬菜与水果中二硫代氨基甲酸盐(酯)类农药残留
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摘要
在密闭加热的顶空瓶中,二硫代氨基甲酸盐(酯)类农药(DTCs)经HCl/SnCl_2溶液消化,反应生成CS_2气体被正己烷吸收,形成CS_2的正己烷溶液,采用气相色谱-质谱(GC-MS)检测CS_2的量,即代表DTCs农药的总残留量。通过蔬菜、水果样品中DTCs农药残留量的测定,对该方法进行了验证。用该方法测定时,CS_2在0. 02～10 mg/L范围内线性良好,相关系数r为0. 9999。福美双的转化率为93. 4%～97. 6%,精密度为1. 5%,符合要求。进行蔬菜、水果样品基质在3个添加水平的回收率实验,平均回收率范围为96. 4%～103. 8%,相对标准偏差为0. 39%～7. 4%。方法检出限为0. 005 mg/kg。
In airtight heating headspace bottle,the dithiocarbamate pesticides( DTCs) were digested to carbon disulfide gas by HCl/SnCl_2 solution. The carbon disulfide were absorbed by hexane,which formed carbon disulfide in hexane solution,and then determined by gas chromatography-mass spectrometry( GC-MS) for further quantification of DTCs pesticide residues. The method was validated by the determination of DTCs pesticide residues in vegetable and fruit samples. With this method,carbon disulfide had good linearity in the range of 0. 02 ～ 10 mg/L( r > 0. 9999). The conversion rates of thiram were within 93. 4% ～ 97. 6%,and the relative standard deviations were1. 5%. The average recoveries at three adding levels in vegetables and fruits matrix were 96. 4%-103. 8% and the relative standard deviations were 0. 39% ～ 7. 4%. The limit of detection was 0. 005 mg/kg.
In airtight heating headspace bottle,the dithiocarbamate pesticides( DTCs) were digested to carbon disulfide gas by HCl/SnCl_2 solution. The carbon disulfide were absorbed by hexane,which formed carbon disulfide in hexane solution,and then determined by gas chromatography-mass spectrometry( GC-MS) for further quantification of DTCs pesticide residues. The method was validated by the determination of DTCs pesticide residues in vegetable and fruit samples. With this method,carbon disulfide had good linearity in the range of 0. 02 ～ 10 mg/L( r > 0. 9999). The conversion rates of thiram were within 93. 4% ～ 97. 6%,and the relative standard deviations were1. 5%. The average recoveries at three adding levels in vegetables and fruits matrix were 96. 4%-103. 8% and the relative standard deviations were 0. 39% ～ 7. 4%. The limit of detection was 0. 005 mg/kg.
引文
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[18] GB 2763-2016,National food safety standard Maximum residue limits for pesticides in food GB 2763-2016,食品安全国家标准食品中农药最大残留限量
[2] Wang J Y,Wang D H,Lu S Y,Cai C P. Chin. J. Food Hyg.,2009,21(6):501王家颖,王丹红,卢声宇,蔡春平.中国食品卫生杂志,2009,21(6):501
[3] Ma J W,Pan C P,Zhang L,Zhang J F. Chin. J. Pestic. Sci.,2010,12(1):22马婧玮,潘灿平,张玲,张军锋.农药学学报,2010,12(1):22
[4] Yang G Q,Yao J R,Zheng Y Q,Dong F S. Modern Agrochem,2005,4(1):6杨桂强,姚建仁,郑永权,董丰收.现代农药,2005,4(1):6
[5] SN/T 1541-2005,Inspection of the total residues of dithiocarbamate pesticides in tea for export SN/T 1541-2005,出口茶叶中二硫代氨基甲酸酯总残留量检验方法
[6] SN 0139-92,Method for determination of dithiocarbamate residues in grain for export SN 0139-92出口粮谷中二硫代氨基甲酸酯残留量检验方法
[7] SN 0157-92,Method for determination of dithiocarbamate residue in fruit for export SN 0157-92出口水果中二硫代氨基甲酸酯残留量检验方法
[8] Shi L L,Shan Z J,Jin Y,Cai D J. J. Instr. Anal.,2005,24(2):92石利利,单正军,金怡,蔡道基.分析测试学报,2005,24(2):92
[9] Pang Z Z,Xue J,Sun H,Wu X B,Xue W,Huang X H. J. Anal. Sci.,2012,28(1):133庞作正,薛健,孙晖,吴晓波,薛雯,黄晓会.分析科学学报,2012,28(1):133
[10] Lu J N,Wang L,Zhang G P,Jiang Z T. Chin. J. Health. Lab. Tec.,2016,26(19):2770鲁晋南,王丽,张国平,蒋忠瑭.中国卫生检验杂志,2016,26(19):2770
[11] Zhang Q P,Wang C M,Ma X Y. Chin. J. Health. Lab. Tec.,2016,26(24):3524张秋萍,王春民,马晓艳.中国卫生检验杂志,2016,26(24):3524
[12] Peng L J,Li L,Wang C Q,Chen D,Wang S H. Yunnan Chem Technol,2017,44(10):32彭丽娟,李苓,王春琼,陈丹,王淑华.云南化工,2017,44(10):32
[13] Zhu W X,Yang J Z,Liu Y F,Wei W. J. Instr. Anal.,2010,29(11):1109祝伟霞,杨冀州,刘亚风,魏蔚.分析测试学报,2010,29(11):1109
[14] Chen W Y,Dong F S,Liu X G,Qin D M,Liao X L,Cheng L,Wang C R,Zheng Y Q. Chinese J. Anal. Chem.,2010,38(4):508陈武瑛,董丰收,刘新刚,秦冬梅,廖晓兰,程莉,王晨蕊,郑永权.分析化学,2010,38(4):508
[15] Ma J W,Dong S J,You W Y,Zhang J P,Niu W M,Pan C P. Chin. J. Pestic. Sci.,2007,9(3):297马婧玮,董姝君,游文宇,张敬平,钮伟民,潘灿平.农药学学报,2007,9(3):297
[16] Wang Y E,Wang J H,Liu R Z,Liu Y M. Journal of Anhui Agri. Sci.,2012,40(31):15252王亚恩,王建华,刘润珠,刘永明.安徽农业科学,2012,40(31):15252
[17] Qin S,Qiao X W,Wang X,Zhao L J. Chinese J. Chromatogr.,2010,28(12):1162秦曙,乔雄梧,王霞,赵丽娟.色谱,2010,28(12):1162
[18] GB 2763-2016,National food safety standard Maximum residue limits for pesticides in food GB 2763-2016,食品安全国家标准食品中农药最大残留限量