高效液相色谱-串联质谱联用技术快速分析水果和蔬菜中毒死蜱及其降解产物
作者:
作者单位:

1.湖北省食品质量安全监督检验研究院,湖北 武汉 430075;2.国家市场监管重点实验室 动物源性食品中重点化学危害物检测技术,湖北 武汉 430075;3.湖北省食品质量安全检测工程技术研究中心, 湖北 武汉 430075

作者简介:

朱正伟 男 工程师 研究方向为食品质量与安全 E-mail:wyzzw0716@163.com

通讯作者:

江丰 男 高级工程师 研究方向为食品质量与安全 E-mail:349136833@qq.com

中图分类号:

R155

基金项目:

国家重点研发计划项目(2018YFC1602300)


Rapid analysis of chlorpyrifos and its degradation products in fruits and vegetables by HPLC-MS/MS
Author:
Affiliation:

1.Hubei Provincial Institute for Food Supervision and Test, Hubei Wuhan 430075, China;2.Key Laboratory of Detection Technology of Focus Chemical Hazards in Animal-derived Food for State Market Regulation, Hubei Wuhan 430075, China;3.Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test, Hubei Wuhan 430075, China

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    摘要:

    目的 建立高效液相色谱-串联质谱联用技术快速分析蔬菜和水果中毒死蜱及其降解产物的检测方法。方法 从色谱和质谱条件两方面对仪器采集参数优化;以韭菜、芹菜、甘蓝、苹果和柑橘为基质,采用QuEChERS方法进行前处理,考察乙二胺-N-丙基硅烷化硅胶和石墨化炭黑(GCB)对毒死蜱及降解产物的影响;最后根据检出限、定量限、线性范围、基质效应、准确度、精密度等对该方法进行考察。结果 流动相为乙腈和0.1%(V/V)甲酸水,质谱采集模式为ESI+,前处理过程中加入GCB 45 mg/5 mL,此时4种目标物在线性范围内线性良好(R2≥0.99),定量限为1~30 μg/kg;在3个加标水平下,回收率为66.1%~113.6%,相对标准偏差为1.3%~16.9%。结论 建立的毒死蜱及降解产物残留量的检测方法快速、高效、准确度和重复性好,适用于蔬菜和水果中毒死蜱及其降解产物的测定。

    Abstract:

    Objective The detection method of rapid analysis of chlorpyrifos and its degradation products in vegetables and fruits by HPLC-MS/MS was established.Methods Both chromatographic conditions and mass spectrometry conditions were optimized. Leek, celery, cabbage, apple and citrus were used as substrates for pretreatment by QuEChERS method, and the effects of PSA and GCB on chlorpyrifos and its degradation products were investigated. Finally, the method was investigated based on limits of detection, limits of quantification, linear range, matrix effect, accuracy and precision.Results The suitable mobile phase was acetonitrile and 0.1% (V/V) formic acid in water. Acquisition parameter of mass spectrometer was ESI+. 45 mg/5 mL of GCB in pretreatment was the best purification condition. The linearity of the four compounds was good (R2≥0.99), and the limits of quantification (LQD) were 1-30 μg/kg. The average recoveries of three levels ranged from 66.1% to 113.6%, and the relative standard deviation (RSD) was 1.3%-16.9%.Conclusion The method is fast, efficient, accurate, repeatable and suitable for the confirmation and quantification of chlorpyrifos and its degradation products in vegetables and fruits.

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朱正伟,吴婉琴,朱松松,陈锂,江丰,范小龙,王会霞.高效液相色谱-串联质谱联用技术快速分析水果和蔬菜中毒死蜱及其降解产物[J].中国食品卫生杂志,2023,35(1):20-26.

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  • 收稿日期:2021-12-31
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  • 在线发布日期: 2023-03-07
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