QuEChERS-液相色谱-串联质谱联用法测定草莓中毒死蜱及其代谢物
目的 建立草莓中毒死蜱及其代谢物残留检测的QuEChERS-液相色谱-串联质谱联用方法。方法 草莓样品用乙腈提取后所得液经过QuEChERS法净化去除杂质。采用5 mmol乙酸铵水-甲醇流动相体系进行洗脱, C18色谱柱进行色谱分离, 电喷雾正负离子模式电离, 多反应监测(multiple-reaction monitoring, MRM), 外标法定量。结果 3,5,6-三氯-2-羟基吡啶(3,5,6-trichloro-2-pyridi-nol, TCP)、毒死蜱、毒死蜱氧和甲基毒死蜱在1.0~200 μg/L浓度范围内线性良好, 相关系数均为0.999, 检出限为0.008~0.279 μg/kg, 定量限为0.026~0.926 μg/kg。在0.010、0.050和0.100 mg/kg 3个浓度水平的平均回收率为71.33%~99.43%, 相对标准偏差在1.51%~5.96%之间。结论 本方法操作简便, 耗时较短, 准确度与精密度较好, 适应性广, 容易形成标准化操作, 可用于草莓样品中毒死蜱及其代谢物残留的分析。
Objective To establish a method for determination of chlorpyrifos and its metabolites in strawberry using QuEChERS-liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods The chlorpyrifos and its metabolites in strawberry were extracted by acetonitrile and purified by QuEChERS. The purified liquid was performed on a C18 column with gradient elution program of 5 mmol ammonium acetate water-methanol. The mass spectrometry was carried out with electrospray ion source in positive and negative mode and multiple reaction monitoring (MRM), and quantified by external standard solution. Results 3,5,6-trichloro-2-pyridi-nol (TCP), chlorpyrifos, chlorpyrifos-oxon and chlorpyrifos-methy had good linear relationships in the range of 1.0~200 μg/L, and the correlation coefficients were 0.999. The limits of detection were 0.008~0.279 μg/kg and the limits of quantitation were 0.026~0.926 μg/kg. The recoveries at 3 spiked levels (0.010, 0.050 and 0.100 mg/kg) were 71.33%~99.43%, with the relative standard deviations of 1.51%~5.96%. Conclusion The established method is simple, convenient, accurate and sensitive, has wide adaptability, and is easy to form standardized operation, which can be used in the analysis of the residues of chlorpyfos and its metabolites in strawberry samples.
标题：QuEChERS-液相色谱-串联质谱联用法测定草莓中毒死蜱及其代谢物
英文标题：Determination of chlorpyrifos and its metabolites in strawberry using QuEChERS-liquid chromatography-tandem mass spectrometry
作者：
李杨 北京农业质量标准与检测技术研究中心,农业部农产品质量安全风险评估实验室(北京)
戴莹 北京市保健品化妆品技术评审中心
马帅 北京农业质量标准与检测技术研究中心,农业部农产品质量安全风险评估实验室(北京)
王蒙 北京农业质量标准与检测技术研究中心,农业部农产品质量安全风险评估实验室(北京)
韩平 北京农业质量标准与检测技术研究中心,农业部农产品质量安全风险评估实验室(北京)
冯晓元 农业部农产品质量安全风险评估实验室北京;北京农业质量标准与检测技术研究中心
中文关键词:草莓,毒死蜱,代谢物,液相色谱-串联质谱法,QuEChERS,
英文关键词:strawberry,chlorpyfos,metabolites,liquid chromatography-tandem mass spectrometry,QuEChERS,
发表日期：2017-07-21
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