采用HPLC-MS/MS法测定黄冠梨中31种农药残留的研究

Determination of 31 Pesticide Residues in Huangguan Pear by HPLC-MS/MS

目的:建立一种同时检测黄冠梨中31种农药残留的高效液相色谱-串联质谱的分析检测方法。方法:采用0.1%甲酸-乙腈为提取液,经C18 150 mg、PSA 200 mg、MgSO4 1 000 mg净化包净化,C18色谱柱分离,乙腈和0.1%甲酸水流动相体系梯度洗脱,在电喷雾正离子化模式下,采用多反应监测(Multi Reaction Monitoring,MRM)检测,外标法定量。结果:31种农药在0.001~0.200μg/mL线性关系良好(R2> 0.991 5),方法检出限为0.000 25~0.025 00 mg/kg,回收率为75.0%~111.5%,相对标准偏差为0.85%~6.70%,并测定了武威市产地黄冠梨样品30批,共检出农药残留8种,其中克百威检出率达67%。结论:该方法处理过程快速、简便、准确及可靠,适用于黄冠梨中31种农药残留的同时检测。

Objective: To establish a method for simultaneous determination of 31 pesticide residue in Huangguan pear by high performance liquid chromatography tandem mass spectrometry. Method: The samples were extracted with 0.1% formic acid and acetonitrile, purified up with C;150 mg, PSA 200 mg, MgSO;1 000 mg purification package, separated by a C;column with acetonitrile and 0.1% formic acid gradient elution in water mobile phase system, detected by multiple reaction monitoring(MRM) in electrospray ionization mode. External standard method for quantification. Result: The pesticide of 31 kinds was in the range of 0.001 ~ 0.200 μg/mL(R2> 0.991 5), and the detection limits were in the range of 0.000 25 ~ 0.025 00 mg/mL. The recoveries ranged from 75.0% to 111.5%and RSD in the range of 0.85% ~ 6.70%.Thirty batches of Huangguan pear samples from three producing areas in Wuwei city were detected, and 8 kinds of pesticide residues were detected, among which the detection rate of Carburyl was 67%. Conclusion: The method is rapid, simple, accurate and reliable, and suitable for simultaneous determination of 31 pesticide residues in Huangguan pear.