分析保护剂对大米中农药残留检测(GC-MS/MS)基质效应补偿作用的评价及应用研究
Evaluation and Application of Analyte Protectants on Matrix Effect Compensation of Pesticide Residue Detection(GC-MS/MS)in Rice
喻玲 1张蕊 2朱琳 2张冰 2张妤 3郭宝元 2王松雪2
作者信息
- 1. 上海理工大学健康科学与工程学院,上海 200093;国家粮食和物资储备局科学研究院,北京 100037
- 2. 国家粮食和物资储备局科学研究院,北京 100037
- 3. 上海理工大学健康科学与工程学院,上海 200093
- 折叠
摘要
研究分别考察了D-山梨糖醇、L-古洛糖酸-γ-内酯、莽草酸和3-乙氧基-1,2-丙二醇4种分析保护剂在气质联用检测大米中农药残留时对基质效应的补偿作用,并采用正交实验对复合分析保护剂进行优化.结果表明:选用保护剂基质标曲定量为最佳定量方式,优化的复合分析保护剂AP3(上机液中D-山梨糖醇、L-古洛糖酸-γ-内酯、莽草酸和3-乙氧基-1,2-丙二醇质量浓度分别为0.2、0.8、0.8、2.0 mg/mL)基质标曲定量,可以有效改善峰形,补偿综合作用良好,各农药标准曲线在2.5～200.0μg/L质量浓度范围内,线性良好,相关系数(R2)均大于0.996,定量限为0.01 mg/kg,10 μg/kg添加水平下,各农药回收率62.2％～117.7％,100、200 μg/kg添加水平下,各农药回收率79.3％～97.1％,满足方法学要求.该法与GB 23200.113-2018对比,47种农药及代谢物回收率结果更好,适用于大批量大米样品中农药筛查和定量检测.
Abstract
In this study,the effects of analyte protectants of sorbitol,L-gulonic acid-γ-lactone,shikimic acid and 3-ethoxy-1,2-propanediol on the matrix effect of pesticide residue analysis in rice by GC-MS were investigated.The mixed analyte protectants were optimized by orthogonal experiments in addition.The quantitative method of protectant matrix calibration was employed.The peak shapes could be effectively improved by using the op-timized mix analyte protectant AP3(0.2 mg/mL sorbitol,0.8 mg/mL L-gulonic acid-γ-lactone,0.8 mg/mL shikimic acid and 2 mg/mL 3-ethoxy-1,2-propanediol in test solution).The linearity was good within the range of 2.5-200.0 μg/L,with the correlation coefficients(R2)higher than 0.996,and the limit of quantitation was 0.01 mg/kg.At the low spiked level(10 μg/kg),the average recoveries of the target pesticides ranged from 62.2％to 117.7％,and at the high spiked levels(100,200 μg/kg),the average recoveries of the target pesticides ranged from 79.3％to 97.1％,meeting the requirements of methodology.The recoveries of 47 pesticides and metab-olites was improved by comparing with the method of GB 23200.113-2018,suitable for qualitative and quantitative detection of pesticides and metabolites residues in large quantities of rice samples.
关键词
分析保护剂/基质效应/大米/农药残留/气相色谱-串联质谱(GC-MS/MS)Key words
analyte protectants/matrix effect/rice/pesticide residues/gas chromatography-Tandem mass spec-trometry(GC-MS/MS)引用本文复制引用
基金项目
国家重点研发计划(十三五)(2019YFC1604805)
行业标准项目(国粮办标[2021]370号)
出版年
2024
NETL
NSTL
万方数据