基于高效液相色谱-四极杆串联飞行时间质谱仪对鸡蛋及制品中氟虫腈的鉴定与测定  

Identification and Determination of Fipronil in Eggs and Qroducts Based on LC-Q-TOF

作　　者：吕飞[1] 黄刚[1] 伍和平[1] 沈鸿[1] 唐艳丽[1] 刘嘉欣 

机构地区：[1]惠州出入境检验检疫局综合技术中心,广东惠州516006

出　　处：《惠州学院学报》2017年第6期20-26,共7页Journal of Huizhou University

摘　　要：利用高效液相色谱分离,四级杆串联飞行时间串联质谱(LC-Q-TOF)鉴定鸡蛋及制品中氟虫腈结构并进行含量测定.经过大量试验,确定用0.1%甲酸乙腈提取,PSA分散固相萃取净化,浓缩,流动相定容.采用Hypersil GOLD C_(18)色谱柱,流动相为甲醇+水,0.2mL/min梯度洗脱,电喷雾离子源(ESl)负离子模式检测.在0.002~0.050 mg/kg范围内,标准曲线回归方程为Y=2.94E+03X+4.67E+03,相关系数为0.998.最低检测限为0.4ug/kg,回收率在65%~108%之间.此法能够对鸡蛋及制品中氟虫腈进行准确结构鉴定与含量测定操作简便、快速、灵敏、准确.LC-Q-TOF was used to identify and determination of the content of fipronil in eggs and products. After a large number of tests, using Hypersil GOLD C1~ ,column determined with 0.1% formic acid acetonitrile extraction, PSA dispersion solid phase extraction purification, concentration, mobile phase volume. The mobile phase was methanol ＋ water, 0.2 mL / min gradient elution, ESI negative ion mode detection. In the range of 0.002- 0.050mg / Kg, the regression curve of the standard curve is Y = 2.94E ＋ 03X ＋ 4.67E ＋ 03, the correlation coefficient is 0.998. The minimum detection limit was 0.4ug / kg, and the recovery was between 65% and 108%. This method can be accurate for the identification and determination of fipronil in eggs and products. The operation is simple, rapid, sensitive and accurate.

关 键 词：高效液相色谱-四极杆串联飞行时间质谱仪 鸡蛋及制品 氟虫腈 结构鉴定 测定 

分 类 号：X836[环境科学与工程—环境工程]