液相色谱-串联质谱法测定牛奶中的己烯雌酚残留量  

Determination of diethylstilbestrol residues in milk by liquid chromatography/tandem mass spectrometry

作　　者：权伍英[1] 郭廓[1] 刘洋[1] QUAN Wuying;GUO Kuo;LIU Yang(Shenyang Center for Dis eos e Control ＆Prevention,She nyang,Liaoning 110031,China)

机构地区：[1]沈阳市疾病预防控制中心,辽宁沈阳110031

出　　处：《河南预防医学杂志》2018年第9期663-665,共3页Henan Journal of Preventive Medicine

摘　　要：目的建立牛奶中己烯雌酚的液相色谱-串联质谱检测方法。方法样品前处理采用QuEChERS萃取技术,阴性样品基质加标外标法,液相色谱-串联质谱电喷雾负离子模式定量检测牛奶中的己烯雌酚。结果己烯雌酚标准溶液的浓度为2.50 ng/m L^50.00 ng/m L时,线性关系良好(r=0.997 2)。己烯雌酚定量检测限为1.00μg/L,添加水平为2.00μg/L,5.00μg/L和10.00μg/L的平均回收率介于85.00%~95.70%之间,相对标准偏差在7.60%~9.80%之间。结论本法快速、灵敏、准确,可用于检测牛奶中的己烯雌酚残留量。Objective To develop a liquid chromatography-tandem mass spectrometry method for the determination of diethylstilbestrol residues in milk. Methods Extraction was carried out using the QuEChERS method while separation.Determination of the target analyte was achieved by liquid chromatography coupled to triple quadrupole mass spectrometry with an electrospray ionization interface operating in negative ion mode and quantified by external standard method using the matrix matched calibration curve. Results When concentration was 2.50 ng/m L-50.00 ng/m L for diethylstilbestrol, the linear relationship was good（r=0.997 2）. The method has a limit of quantification of 1.00 μg/L.The mean recovery ranged from 85.00 % -95.70 % at three levels for 2.0 0 μg/L,5.00 μg/L, 10.00 μg/L and the relative standard derivations were between 7.60 % and 9.80 %. Conclusions The method is quick, sensitive and specific for determination of diethylstilbestrol residues in milk.

关 键 词：液相色谱-串联质谱法 QUECHERS 己烯雌酚 牛奶 

分 类 号：TS207.5[轻工技术与工程—食品科学]