1. 福建中检华日食品安全检测有限公司
2. 宁德出入境检验检疫局
3. 福建出入境检验检疫局
4. 中国检验认证集团福建有限公司
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苏建峰, 钟茂生, 陈晶, 等. 气相色谱-质谱法与气相色谱法测定茶叶及茶叶加工品中295种农药多残留[J]. 分析测试学报, 2015,34(6):625-638.
Multi-residue Determination of 295 Pesticides in Tea and Its Products by Gas Chromatography-Mass Spectrometry and Gas Chromatography[J]. 2015,34(6):625-638.
建立了一种适用于茶叶及茶叶加工品(超微茶粉、速溶茶粉)中农药多残留分析的前处理方法(方法Ⅰ),配以一个辅助方法(方法Ⅱ),构成茶叶及茶叶加工品中常见有机磷类、有机氯类、拟除虫菊酯类、氨基甲酸酯类及其它杂类共295种农药多残留的分析体系(方法Ⅰ286种,方法Ⅱ9种)。方法Ⅰ中,样品用乙酸乙酯均质和超声波提取,提取液利用丙酮的溶解性能和亲水亲脂特性,使待测农药溶于少量丙酮中并借丙酮在水相与正己烷相之间的转移实现了待测农药的选择性转移,从而除去茶多酚、咖啡因、蛋白质、有机酸、矿物质、糖类及调味组分等大部分杂质,然后采用Cleanert TPT柱除去色素和剩余的少部分极性杂质,气相色谱-质谱(GC-MS)进行分析;方法Ⅱ中,样品采用乙腈均质和超声波提取,提取液经Cleanert TPT柱净化后供气相色谱(GC)分析。GC-MS采用选择离子监测方式(SIM),GC采用火焰光度检测器(FPD),外标法定量。在最优条件下,方法的线性范围为0.01~1.00 mg/L,r2>0.99,定量下限(S/N≥10)为0.01~0.10 mg/kg。加标水平为0.10 mg/kg时,方法Ⅰ回收率为51%~135%,其中回收率在70%~110%之间的占88.3%,相对标准偏差为3.7%~18%;方法Ⅱ回收率为68%~99%,相对标准偏差为3.5%~8.2%。该方法简便、准确、灵敏、快速,可满足茶叶及茶叶加工品中多种农药残留的检测要求。
A method was developed and applied to determine the residual amounts of 286 pesticides(organophosphorus,organochlorine,pyrethroid,carbamate and other pesticides) in tea and its products by gas chromatography-mass spectrometry(method Ⅰ),and an other method was applied to determine 9 kinds of strongly polar organophosphorus pesticides in tea and its products by gas chromatography(method Ⅱ).For method Ⅰ,the residues were extracted from homogenized tissue with ethyl acetate assisted by ultrasonication.The clear supernatant liquid purified by solvent transfer technique and solid phase extraction(Cleanert TPT column) was ready for GC-MS analysis.For method Ⅱ,the residues were extracted from homogenized tissue using acetonitrile assisted by ultrasonication.The supernatant was purified by solid phase extraction(Cleanert TPT column) prior to GC analysis.Determinations were performed by GC-MS in selected ion monitoring(SIM) mode and GC method with flame photometric detector(FPD),then external standard method was used in the quantification.The methods were convenient and rapid after the conditions of pretreatment and determination were investigated.Under the optimal conditions,the quantitation limits of two methods(S/N≥10) for pesticides were in the range of 0.01-0.10 mg/kg.The linear ranges were between 0.01 mg/L and 1.00 mg/L with correlation coefficients(r2) larger than 0.99.Tests for recovery were carried out by addition of standards at concentration of 0.10 mg/kg,the recoveries of method I were in the range of 51%-135%,among which the recoveries for 88.3% pesticides were between 70% and 110%,and the recoveries of method Ⅱ were in the range of 68%-99%,while the relative standard deviations were in the ranges of 3.7%-18% and 3.5%-8.2%,respectively.The methods are easy,fast and sensitive,and could meet the requirements of the multiresidual analysis in tea and its products.
气相色谱法气相色谱-质谱法样品前处理农药多残留分析茶叶茶粉
gas chromatography(GC)gas chromatography-mass spectrometry(GC-MS)sample pretreatmentmultiresidual analysisteatea powder
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