PRiME HLB-超高效液相色谱串联质谱法测定原料乳中31种药物残留  

Determination of 31 Drug Residues in Raw Milk by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry Based on PRiME-HLB

作　　者：韩瑨烜 其布日其其格 韩丽 李强 HAN Jinxuan;QI Buriqiqige;HAN Li;LI Qiang(Xinjiang Uygur Autonomous Region Product Quality Supervision and Inspection Institute,Urumqi 830000,China;Xinjiang Tianrun Biotechnology Co.,Ltd.,Urumqi 830088,China)

机构地区：[1]新疆维吾尔自治区产品质量监督检验研究院,新疆乌鲁木齐830000 [2]新疆天润生物科技股份有限公司,新疆乌鲁木齐830088

出　　处：《食品科技》2024年第7期315-321,共7页Food Science and Technology

基　　金：新疆生产建设兵团十二师科技计划项目(SRS2022008)。

摘　　要：文章建立了基于PRi ME HLB(Hydrophilic lipophilic balance)-超高效液相色谱串联质谱法对原料乳中31种兽药的快速筛查方法。样本经1%甲酸-乙腈提取,超声波水浴20 min,震荡涡旋5 min助提,离心后取上清液过PRi ME HLB固相萃取柱净化,浓缩至近干后用10%甲醇-水溶液复溶。以Hypersil GOLD C18为分离柱,0.1%甲酸-水/甲醇为流动相,梯度洗脱,电喷雾离子源正离子多反应监测模式下分析。采用该方法,31种药物总分析时长仅为10 min,各组分离子色谱图峰形良好,保留时间在1.5~9.0 min之间。各组分质量浓度在10~200μg/kg线性范围内判定系数(R2)均大于0.99,检出限为0.5~20.0μg/kg,定量限为5.0~80.0μg/kg。在80、40、20μg/kg 3个加标水平下,31种药物回收率为62.4%~99.8%,相对标准偏差均小于10%(n=6)。该方法具有操作简便、分析快速、基质干扰小等优点,适用于原料乳中多种兽药的高通量快速筛查。A method for the determination of 31 kinds of veterinary drugs in raw milk by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)based on PRiME-HLB(Hydrophilic lipophilic balance).The samples were extracted by 1%formic acid-acetonitrile,ultrasoniced for 20 min and oscillating vortex for 5 min.After centrifugation,the supernatant was purified through a PRiME HLB solid phase extraction column,concentrated to near dryness,and re-dissolved in 10%methanolwater solution.Separation was achieved using a Hypersil GOLD C18 column with 0.1%formic acid-water/methanol as the mobile phase in gradient elution,and analysis was performed in the electron spray ionization(ESI)positive ion multiple reaction monitoring(MRM)mode.Under the optimized conditions,the total analysis time of 31 drugs was only 10 min,and the peak shape of ion chromatogram of each group was good,the retention time was between 1.5-9.0 min.The correlation coefficients(R2)for the linear range of mass concentrations between 10μg/kg and 200μg/kg were all greater than 0.99.The limit of detection and limit of quantification were 0.5-20.0μg/kg and 5.0-80.0μg/kg,respectively.At three spiked levels of 80,40,and 20μg/kg,the recovery rates of the method were in the range of 62.4%-99.8%.The relative standard deviations were less than 10%(n=6).The method has the advantages of simple operation,fast analysis and little matrix interference,and is suitable for high-throughput screening of various veterinary drugs in raw milk.

关 键 词：超高效液相色谱串联质谱法 PRi ME HLB 原料乳 兽药残留 快速筛查 

分 类 号：TS207.5*3[轻工技术与工程—食品科学]