RSPE-UPLC-MS/MS法测定禽蛋中氯羟吡啶残留  

Determination of the clopidol residues in poultry eggs by RSPE-UPLC-MS/MS

作　　者：梁飞燕 林小莹 辛丽娜 叶勇[2] 陈圣杰 王捷[2] LIANG Fei-yan;LIN Xiao-ying;XIN Li-na;YE Yong;CHEN Sheng-jie;WANG Jie(Guangxi-ASEAN Food Inspection Center, Nanning 530021, China;College of Pharmacy, Guangxi Medical University, Nanning 530021, China)

机构地区：[1]广西东盟食品检验检测中心,广西南宁530021 [2]广西医科大学药学院,广西南宁530021

出　　处：《广西大学学报（自然科学版）》2020年第6期1492-1497,共6页Journal of Guangxi University（Natural Science Edition）

基　　金：广西食品药品监督管理局直属单位食品药品安全科研项目计划(桂食药科2018-9);广西南宁市科学研究与技术开发计划项目(20173158-3);广西南宁市青秀区科学研究与技术开发计划项目(2015Z01)。

摘　　要：建立反相固相萃取(RSPE)-超高效液相色谱(UPLC)-串联质谱(MS/MS)法考察禽蛋中氯羟吡啶的残留现状。样品用乙腈∶水(90∶10,v/v)提取,Oasis PRIME HLB反固相萃取柱(500 mg,6 cc)纯化,乙腈∶水(10∶90,v/v)复溶,CAPCELL PAK C18 MGⅢ-H色谱柱(3μm,2.0 mm×100 mm)进行分离,0.1%甲酸溶液乙腈梯度洗脱,正离子多反应监测。结果表明:氯羟吡啶在0.5~20 ng/mL呈良好线性关系,相关系数为0.9992;检出限和定量限分别为0.0013、0.0045μg/kg;在0.4、1.0、4.0μg/kg三种不同浓度的平均回收率分别为105.90%、106.82%、101.65%,RSD分别为1.53%、1.11%、2.91%。该方法具有简单、快速、准确、灵敏的优点,可用于禽蛋中氯羟吡啶残留的测定。A method of reversed-phase solid phase extraction-ultra high performance liquid chromatography-tandem mass spectrometry was established for investigating the status of clopidol residues in poultry eggs.Samples were extracted by acetonitrile:water(90∶10,v/v),purified by the Oasis PRIME HLB reversed-phase solid phase column(500 mg,6 cc),redissolved by acetonitrile:water(10∶90,v/v),and separated by CAPCELL PAK C18 MGⅢ-H column(3μm,2.0 mm×100 mm),gradiently eluted with 0.1%formic acid solution and acetonitrile,monitored by positive ion multi-reaction.The results show that the standard curve of clopidol showed a good linear relationship in the range of 0.5~20 ng/mL,and the correlation coefficient was 0.9992.The detection limit and quantitative limit were 0.0013μg/kg and 0.0045μg/kg,respectively.The average recoveries at 3 different levels of 0.4,1.0,4.0μg/kg were 105.90%,106.82%,and 101.65%,respectively,and the RSD were 1.53%,1.11%,and 2.91%,respectively.This method has the advantages of simplicity,speed,accuracy and sensitivity,and can be used for the determination of clopidol residues in poultry eggs.

关 键 词：禽蛋 氯羟吡啶 兽药残留分析 

分 类 号：R917[医药卫生—药物分析学]