摘要
目的:考察基质效应对菊花中农药残留检测结果准确性的影响。方法:采用气相色谱-质谱联用(GC-MS/MS)和液相色谱-质谱联用(LC-MS/MS)法对不同产地菊花饮片中的禁用农药进行检测。GC-MS/MS采用DM-17MS柱(30 m×0.25 mm,0.25μm),载气为高纯氦,程序升温,电子轰击源(EI)检测;LC-MS/MS采用Agilent SB-C_(18)(10 cm×2.7 mm,2.1μm)色谱柱,以0.1%甲酸溶液(含5 mmol·L^(-1)甲酸铵)为流动相A,以95%乙腈溶液(含5 mmol·L^(-1)甲酸铵和0.1%甲酸)为流动相B,梯度洗脱,电喷雾(ESI)离子源检测。考察不同前处理方式下(直接提取法、QuEChers法和固相萃取法)样品基质、不同基质浓度(0.2 g·mL^(-1)或0.5 g·mL^(-1))等对农残检测结果的影响。结果:在菊花的禁用农药检测过程中,超过40%的农药指标表现为强基质效应。通过降低样品基质浓度可以有效降低基质效应并减少不同菊花80%以上农药指标的基质效应差异。不同前处理方式对于多数指标的基质效应强弱并无明显改善,但可以减少基质对仪器的污染。在日常检测时应采用基质匹配的方法进行定量,以降低基质效应给检测准确性带来的影响。结论:在菊花农药残留检测时基质效应不可忽略,降低样品基质浓度可有效降低测定时基质效应差异对检测结果的影响。本研究为提高中药农药测定方法准确性提供参考。
Objective:To investigate the influence of matrix effect on the accuracy of detection of pesticide residue in Chrysanthemum.Methods:Gas chromatography-mass spectrometry(GC-MS/MS)and liquid chromatography-mass spectrometry(LC-MS/MS)were used to detect the banned pesticides in chrysanthemum decoction pieces from different habitats.GC-MS/MS was performed on a DM-17MS column(30 m×0.25 mm,0.25μm)with high-purity helium as the carrier gas,temperature programmed,and detected by electron impact source(EI);LC-MS/MS was performed on an Agilent SB-C_(18) column(10 cm×2.7 mm,2.1μm)with 0.1%formic acid solution(containing 5 mmol·L^(-1) ammonium formate)as mobile phase A and 95%acetonitrile solution(containing 5 mmol·L^(-1) ammonium formate and 0.1%formic acid)as mobile phase B.Gradient elution and electric spray(ESI)ion source detection were performed.The effects of sample matrix(direct extraction,QuEChers,and solid-phase extraction)and different matrix concentrations(0.2 g·mL^(-1) or 0.5 g·mL^(-1))on the detection results of pesticide residues under different pretreatment methods were investigated.Results:In the detection process of banned pesticides in Chrysanthemum,over 40%pesticides showed strong matrix effect.By reducing the matrix concentration of the sample,the matrix effect could be effectively reduced and the matrix effect difference of pesticides by more than 80%among different batches of Chrysanthemum could be reduced.Different pretreatment methods had no significant improvement in the matrix effect of most indicators,but could reduce the pollution of the matrix to the instrument.In order to reduce the influence of matrix effect on the accuracy of determination,matrix matching method should be used in daily detection.Conclusion:Matrix effect cannot be ignored in the detection of pesticides in Chrysanthemum and reducing the sample matrix concentration can effectively reduce the impact of matrix effect differences on the detection results,which provides a reference for improving the accuracy of pesticide detection method of traditional Chinese medicine.
作者
刘芫汐
韩晶
程韬
王莹
金红宇
魏锋
Liu Yuanxi;Han Jing;Cheng Tao;Wang Ying;Jin Hongyu;Wei Feng(National Institutes for Food and Drug Control,Beijing 102629,China;Jilin Institute for Drug Control,Changchun 130033,China;Guizhou Institute for Food and Drug Control,Guiyang 550000,China)
出处
《中国药事》
2025年第6期662-672,共11页
Chinese Pharmaceutical Affairs
基金
国家重点研发计划项目基于限量控制的安全性快速检测技术(编号2023YFC3504103)
中国食品药品检定研究院中青年发展研究基金(编号2024A6)
国家重点研发计划:生态种植药材品质多维评价及价值评估(编号2022YFC3501505)。
关键词
菊花
农药残留
基质效应
直接提取法
QuEChers法
固相萃取法
Chrysanthemum
pesticide residues
matrix effect
direct extraction method
QuEChers method
solid phase extraction method
