超高效液相色谱—串联质谱法测定生鲜乳中6种农药的残留

Determination on 6 Kinds of Pesticide Residues in the Raw Milk by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

本试验建立了生鲜乳中西草净、枯草隆、西码津、莠去津、乙草胺和丁草胺残留量的超高效液相―串联质谱检测方法。牛奶样品用乙腈提取,经固相萃取柱净化,C18色谱柱分离,以0.1%(V/V)甲酸―水/乙腈为流动相,采用梯度洗脱方式进行液相色谱分离,多反应监测模式,外标法进行定量。结果发现,西草净、枯草隆、西码津、莠去津、乙草胺和丁草胺的检测限分别为0.1、1.0、0.2、0.1、4.0和4.0μg/L,线性范围分别为1.0~50.0、10.0~500.0、1.0~50.0、1.0~50.0、20.0~1000.0和20.0~1000.0μg/L。表明该方法专属性强、灵敏度高、分离度好,适用于生鲜乳中西草净、枯草隆、西码津、莠去津、乙草胺和丁草胺残留量的测定。

The author established a kind of method to check the residues of simetryn,chloroxuron,simazine,atrazine,acetochlor,butachlor in milk.The samples were extracted by acetonitrile,purified by solid phase extraction,and were determined by an ACQUITY UPLCTM BEH C18column with gradient elution using acetonitrile and water(containing 0.1%formic acid)as mobile phase.The mass spectrometric acquisitions were carried out by means of multiple reaction monitoring(MRM)in electrospray positive ionization mode.The detection limits of simetryn,chloroxuron,simazine,atrazine,acetochlor,butachlor were0.1,1.0,0.2,0.1,4.0and 4.0μg/L.The calibration curves were liner from 1.0~50.0,10.0~500.0,1.0~50.0,1.0~50.0,20.0~1000.0and 20.0~1000.0μg/L.The results showed that this method had specific,sensitive,and suitable for determination on simetryn,chloroxuron,simazine,atrazine,acetochlor,butachlor in the milk.