LC-MS/MS法同时测定穿心莲中6种农药残留量

Simultaneous Determination of 6 Pesticide Residues in Andrographis paniculata by LC-MS/MS

本研究旨在建立测定穿心莲中6种农药残留量的方法,更好地控制药材质量。研究通过高效液相色谱-串联四极杆质谱仪以多反应监测(MRNI)的扫描模式对空白、样品和对照品进行测试,采用ACQUITY UPLC BEHC18柱分离,高效液相色谱-串联质谱联用方法测定穿心莲中常用的6种农药残留量。结果表明:该方法下霜脲氰、敌敌畏、2,4-滴、精喹禾灵、毒死蜱和氯氰菊酯的检测限分别为0.015 mg/kg、0.125 mg/kg、0.04 mg/kg、0.01 mg/kg、0.03 mg/kg、0.025 mg/kg,在一定浓度范围内,响应值与质量浓度的线性关系良好(r> 0.990),6种目标物对照品溶液及样品加标溶液在仪器参数波动时结果RSD均小于10%。室温下,6种目标物对照品溶液及样品加标溶液在14h内峰面积RSD均小于5%,在14h内溶液稳定。20批穿心莲样品检测结果:仅其中1批检出氯氰菊酯41.2ng/g,其余样品均未检出,符合要求。本研究方法简便,线性、耐用性良好,能满足同时测定6种农药在穿心莲中的残留量。

The aim of this study was to establish a method for the determination of 6 pesticide residues in Andrographis paniculata,so as to better control the quality of the medicinal materials.A high-performance liquid chromatography-tandem quadrupole mass spectrometer was used to test blank,sample and control samples in the scanning mode of multi-reaction monitoring(MRNI).ACQUITY UPLC BEH C18 column was used for separation,and high performance liquid chromatography-tandem mass spectrometry was used to determine the 6 pesticide residues commonly used in Andrographis paniculata.The results showed that the detection limits of cypermethrin,dichlorvos,2,4-drops,glyphosate,chlorpyrifos,and cypermethrin under this method were 0.015 mg/kg,0.125 mg/kg,0.04 mg/kg,0.01 mg/kg,0.03 mg/kg,and 0.025 mg/kg,respectively.Within a certain concentration range,the response values had a good linear relationship with the mass concentration(r>0.990),and the RSD of the six target substance reference solutions and sample spiked solutions were all less than 10%when the instrument parameters fluctuated.At room temperature,the RSD of the peak area of the six target reference solution and sample spiking solution was less than 5%within 14 hours,and the solution remained stable within 14 h.The test results of 20 batches of Andrographis paniculata samples showed that only one batch detected 41.2 ng/g of cypermethrin,while the remaining samples were not detected,meeting the requirements.This research method is simple,linear and durable,and can be used to determine the residues of six pesticides in Andrographis paniculata at the same time.