高效液相色谱-串联质谱法同时测定谷物中10种HPPD抑制剂类除草剂及其代谢物

Determination of 10 HPPD inhibitors and a metabolite in cereals by HPLC-MS/MS

边海涛 ¹董睿男 ¹勇艳华 ¹李鹏 ¹苏春敏 ¹刘杨¹

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作者信息

1. 大连市检验检测认证技术服务中心国家市场监管技术创新中心(食用农产品安全快速检测与追溯),辽宁大连 116630
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摘要

[目的]建立高效液相色谱-串联质谱法同时测定谷物(小麦、玉米、糙米)中10种HPPD抑制剂类除草剂及其代谢物的方法.[方法]样品经体积分数为3％甲酸水溶液浸润,乙腈提取,乙二胺-N-丙基硅烷和十八烷基硅烷键合硅胶净化,高效液相色谱-串联质谱测定.[结果]10种HPPD抑制剂类除草剂及其代谢物在1.5～100 μg/L质量浓度范围内呈现良好的线性关系,定量限为0.01 mg/kg,3个添加水平(0.01、0.03、0.1 mg/kg)下,在3种谷物基质中平均回收率为74.3％～112.7％,相对标准偏差小于8.7％.[结论]该方法简便高效、准确度高、精密度好,适用于谷物中10种HPPD抑制剂类除草剂及其代谢物的测定.

Abstract

[Aims]A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method was established for simultaneous determination of 10 4-hydroxyphenylpyruvate dioxygenase(HPPD)inhibitor herbicides and a metabolite in cereals(wheat,corn and brown rice).[Methods]The samples were soaked by 3％formic acid aqueous solution(volume fraction),extracted by acetonitrile,purified by primary secondary amine(PSA)and octadecylsilane(C18),and detected by HPLC-MS/MS.[Results]Good linear relationship appeared in the mass concentration range of 1.5-100 pg/L for 10 HPPD inhibitor herbicides and the metabolite.The limits of quantitation(LOQs)of them were 0.01 mg/kg.At three spiked levels of 0.01,0.03 and 0.1 mg/kg,the average recoveries were 74.3％-112.7％in 3 cereal matrices,with relative standard deviations(RSDs)less than 8.7％.[Conclusions]The method is simple and effective,with high accuracy and good precision,which is suitable for determination of the ten HPPD inhibitor herbicides and the metabolite in cereals.

关键词

高效液相色谱-串联质谱法/HPPD抑制剂/除草剂/谷物/残留

Key words

high performance liquid chromatography-tandem mass spectrometry/4-hydroxyphenylpyruvate dioxygenase inhibitor/herbicide/cereal/residue

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基金项目

国家市场监督管理总局科技项目(2020MK114)

出版年

2024

农药

沈阳化工研究院有限公司

农药

CSTPCDCSCD北大核心

影响因子：0.665

ISSN：1006-0413

参考文献量19

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