UPLC-MS/MS法测定猪粪中赛庚啶和可乐定残留量的研究  

Study on the determination of cyproheptadine and clonidine residues in pig manure by UPLC-MS/MS method

作　　者：张婧 王博 严凤 吴剑平 潘娟 陈晶[2] ZHANG Jing;WANG Bo;YAN Feng;WU Jianping;PAN Juan;CHEN Jing(Shanghai Institute of Veterinary Drug and Feed Supervision,Shanghai 201103,China;Shanghai Vocational College of Agriculture and Forestry,Shanghai 201699,China)

机构地区：[1]上海市兽药饲料检测所,上海201103 [2]上海农林职业技术学院,上海201699

出　　处：《黑龙江畜牧兽医》2021年第16期120-125,共6页Heilongjiang Animal Science And veterinary Medicine

基　　金：上海农林职业技术学院中青年领军人才培养项目(A2-0273-20-01-01);上海市市级农口系统青年人才成长计划项目(沪农青字[2017]第2-4号)。

摘　　要：为了拓宽赛庚啶和可乐定残留的监测环节,更好地监控粪污还田再利用过程中药物排放情况,试验将猪粪便样品用0.1 mol/L盐酸-甲醇(1:1,V/V)溶液提取及MCX固相萃取柱净化后,采用超高效液相色谱-串联质谱(UPLC-MS/MS)法检测,并以二苯拉林及盐酸可乐定-D4分别作为赛庚啶和可乐定的内标物进行内标法定量,绘制标准曲线,考察所建立方法的灵敏度、准确度及精密度,同时用建立的方法对临床采集的30批猪粪便样品进行检测。结果表明:赛庚啶和可乐定浓度在0.5~100 ng/mL范围内线性关系良好(R^(2)>0.9900),在5,10,20μg/kg添加水平下,猪粪便中赛庚啶和可乐定的回收率分别为99.5%~116.5%和97.3%~116.0%,相对标准偏差(RSD)均<10%,检测限和定量限分别为1,5μg/kg。30批猪粪样品中并未检出赛庚啶或可乐定残留。说明该方法灵敏、准确,可作为猪粪便中赛庚啶和可乐定检测的确证方法,用于完善两种药物的监测体系。In order to broaden the monitoring link of cyproheptadine and clonidine residues,and to better supervise the discharge of drugs in the process of returning manure to the field for reuse,in the experiment,pig manure samples were extracted with 0.1 mol/L hydrochloric acid-methanol(1:1,V/V)solution and purified by MCX solid phase extraction column;ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was used for detection,and diphenylpyraline and Clonidine-D4 were used as internal standards for cyproheptadine and clonidine for internal standard quantification,with drawing a standard curve,and examining the sensitivity,accuracy and precision of the established method,the established method was used to detect 30 batches of pig manure samples collected clinically.The results showed that the concentration of cyproheptadine and clonidine had a good linear relationship in the range of 0.5-100 ng/mL(R^(2)>0.9900);at the levels of 5,10,20μg/kg,the recoveries of cyproheptadine and clonidine in pig manure were 99.5%-116.5%and 97.3%-116.0%,respectively;the relative standard deviations(RSD)were both<10%;the limit of detection and limit of quantification were 1,5μg/kg,respectively.No cyproheptadine or clonidine residues were detected in 30 batches of pig manure samples.The results suggested that the method was sensitive and accurate,and could be used as a confirmation method for the detection of cyproheptadine and clonidine in pig manure,and further improved the monitoring system of the two drugs.

关 键 词：赛庚啶 可乐定 超高效液相色谱-串联质谱(UPLC-MS/MS) 猪 粪便 残留 

分 类 号：S859.7[农业科学—临床兽医学]