分散固相萃取-超高效液相色谱-三重四极杆质谱法快速检测奶粉中16种喹诺酮药物残留  

Rapid Determination of 16 Quinolones Residues in Milk Powder by Dispersive Solid Phase Extraction Ultra Performance Liquid Chromatography Triple Quadrupole Mass Spectrometry

作　　者：李涛 周艳华[2] 向俊 徐文泱 孙桂芳 LI Tao;ZHOU Yanhua;XIANG Jun;XU Wenyang;SUN Guifang(Hunan Institute of Commodity Quality Inspection,Hunan Provincial Key Laboratory of Food Safety Monitoring and Early Warning,Changsha 410011,China;Changsha Environmental Protection College,Changsha 410004,China)

机构地区：[1]湖南省产商品质量检验研究院,食品安全监测与预警湖南省重点实验室,长沙410111 [2]长沙环境保护职业技术学院,长沙410004

出　　处：《中国乳品工业》2021年第11期54-58,64,共6页China Dairy Industry

基　　金：湖南创新型省份建设专项(2020SK2128);湖南省科技创新平台与人才计划项目(2019TP1058)。

摘　　要：建立了一种分散固相萃取-超高效液相色谱-三重四级杆质谱(DSPE-UPLC-MS/MS)同时检测奶粉中16种喹诺酮类药物残留的快速检测方法。奶粉经水和1%甲酸乙腈提取后,通过C18吸附剂和PSA吸附剂净化后,经C18色谱柱分离,三重四级杆质谱仪检测。结果表明:16种喹诺酮在2.0~100.0 ng/mL范围内具有良好的线性关系(R2≥0.997)。该方法 16种喹诺酮检出限范围为0.03~0.4μg/kg,定量限范围为0.1~1.5μg/kg。16种喹诺酮的加标回收率在78.1%~105.3%之间,相对标准偏差RSD在0.9%~8.8%之间。该方法简单高效、准确度高,可作为乳粉中喹诺酮类药物残留的定量检验方法。A method for the simultaneous rapid determination of the residues of 16 quinolones in milk powder by dispersive solid phase extraction(DSPE)and ultra performance liquid chromatographytandern mass spectrometry(UPLC-MS/MS) was established. Milk powder was extracted by water and 1% formic acid acetonitrile, purified by C18 adsorbent and PSA adsorbent, separated by C18 column and detected by triple quadrupole mass spectrometer. The linearity of all the 16 quinolones in the range from 2.0 to 100.0 ng/mL had correlation coefficients greater than 0.997. The limits of detection(LOD) of the method were from 0.03 to 0.4μg/kg and the limits of quantification(LOQ)were from 0.1 to 1.5μg/kg. The average recoveries of the 16 quinolones were in the range from 78.1% to 105.3%, with the precursorions(n=6)in the range of 0.9%-8.8%. The method is simple, efficient and accurate, and can be used for the quantitative confirmation of quinolones residues in milk powder.

关 键 词：分散固相萃取 超高效液相色谱-三重四级杆质谱 喹诺酮类化合物 乳粉 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程]