摘要
目的建立超高效液相色谱-串联质谱法同时检测铁皮石斛中32种农药残留的方法,并监测市场上铁皮石斛的农药残留。方法样品经乙腈提取净化后,采用Acquity BEH C_(18)色谱柱分离,以0.1%甲酸溶液-乙腈为流动相进行梯度洗脱,外标法定量。对铁皮石斛主产区3种样品进行农药检测。结果32种农药在一定范围内线性关系良好,相关系数r≥0.9968,检出限为0.1~0.5μg/kg。在不同添加水平下,各基质中超过30种农药的回收率在70%~110%之间,相对标准偏差小于20%。3种石斛样品仅发现1个鲜样中苯醚甲环唑残留量(2.69 mg/kg)超过GB 2763—2021《食品安全国家标准食品中农药最大残留限量》规定最大残留限量(1 mg/kg),合格率为98%。其中烯酰吗啉、吡唑醚菌酯、精甲霜灵、苯醚甲环唑和戊唑醇5种农药检出率较高。结论本方法灵敏度高,可作为铁皮石斛中农残的快速筛查和定量分析。所抽检的3种铁皮石斛样品中农药种类检出较多,而残留中值较低。本研究为铁皮石斛的质量安全控制提供技术支撑。
Objective To establish a method for simultaneous detection of 32 kinds of pesticide residues in Dendrobium officinale by ultra performance liquid chromatography-tandem mass spectrometry and monitor pesticide residues in Dendrobium officinale on the market.Methods The sample was extracted with acetonitrile,purified,and separated using an Acquire BEH C_(18) chromatographic column.Gradient elution was performed using a 0.1%formic acid-acetonitrile as the mobile phase,and quantitative analysis was performed using an external standard method.Pesticide monitoring was carried out on the 3 kinds of samples from the Dendrobium officinale main production areas.Results The linear relationships of 32 kinds of pesticides were good in a certain range,the correlation coefficients r≥0.9968,the limits of detection were 0.1-0.5μg/kg.At different levels of addition,the recoveries of over 30 kinds of pesticides in each substrate ranged from 70%-110%,the relative standard deviations were less than 20%.Among the 3 types of Dendrobium officinale samples,only 1 fresh sample was found to have a residue level of difenoconazole(2.69 mg/kg)exceeding the maximum residue limit in GB 2763—2021 National standards for food safety-Maximum residue limits for pesticides in food(1 mg/kg),with a qualification rate of 98%.Among them,the detection rates of 5 kinds of pesticides,namely enoylmorpholine,pyrazolidinolate,metformin,difenoconazole,and tebuconazole,were relatively high.Conclusion This method has high sensitivity and can be used for rapid screening and quantitative analysis of pesticide residues in Dendrobium officinale.There are more kinds of pesticides in 3 kinds of samples of Dendrobium officinale,but the median residue is lower.This study provides technical support for the quality and safety control of Dendrobium officinale.
作者
凌淑萍
付岩
王全胜
张亮
吕燕
吴银良
LING Shu-Ping;FU Yan;WANG Quan-Sheng;ZHANG Liang;LV Yan;WU Yin-Liang(Ningbo Academy of Agricultural Science,Ningbo 315040,China;Ningbo Key Laboratory of Testing and Control for Characteristic Agro-product Quality and Safety,Ningbo 315040,China)
出处
《实验室检测》
2023年第6期24-35,共12页
Laboratory Testing
基金
宁波市公益性科技计划项目(2021S074)
关键词
铁皮石斛
农药
膳食风险评估
超高效液相色谱-串联质谱法
Dendrobium officinale
pesticides
dietary risk assessment
ultra performance liquid chromatography-tandem mass spectrometry
