SPE-UPLC-MS/MS法测定牛奶中β-内酰胺类药物残留  

Determination of β-lactams residues in milk by SPE-UPLC-MS/MS

作　　者：孙涛[1] 刘圣红[1] 刘河疆[1] 古丽斯坦[1] 安静[1] 王成[1] Sun Tao Liu Shenghong Liu He- jiang Gulisitan An Jing Wang Cheng(Institute of Quality Standards ＆ Testing Technology for Agro-Products , XinJiang Academy of Agricultural Science, Laboratory of Quality and Safety Risk Assessment for agro-Products （Urumqi ）, Key Laboratory of agro-Products Quality and Safety of Xin- jiang , Urumqi 830091,China)

机构地区：[1]新疆农业科学院农业质量标准与检测技术研究所/农业部农产品质量安全风险评估实验室(乌鲁木齐)/新疆农产品质量安全实验室,乌鲁木齐830091

出　　处：《分析仪器》2017年第1期7-12,共6页Analytical Instrumentation

基　　金：自治区公益性科研院所基本科研项目(KYGY2016094);2016年生鲜乳农兽药;重金属和生物毒素等危害因子摸底排查与验证评估项目(GJFP201600802)

摘　　要：本试验应用固相萃取技术(SPE),结合超高效液相色谱-串联质谱联用仪(UPLC-MS/MS),建立了快速测定生鲜乳中!-内酰胺类药物残留的方法。样品经乙腈提取,Oaiss PRiME HLB固相萃取小柱净化后,以0.1%甲酸乙腈溶液和0.1%水溶液为流动相,Waters C_(18)色谱柱进行分离;多反应监测(MRM)模式,外标法进行定量。方法回收率在70.1%~95.5%之间;相对标准偏差(n=3)范围为1.0%~9.1%;线性范围为0.002~0.100mg/L;检出限为0.1~0.6μg/kg;定量限为0.3~1.8μg/kg。表明该方法专属性强、灵敏度高,适用于生鲜乳中β-内酰胺类药物残留的测定。The samples were extracted by acetonitrile and purified with Oaiss an PRIME HLB car-tridge. The UPLC analyses were performed on an Acquity UPLC C18 column with gradient elution using acetonitrile（containing 0.1% formic）and water（containing 0.1% formic） as mobile phase. The mass spec- trometric acquisitions were carried out by means of multiple reaction monitoring（MRM） in electrospray positive ionization mode. The average recoveries of β-lactams antibiotics ranged from 70.1% to 95.5 %, with the relative standard deviation from 1.0% to 9.1%, the calibration curve was liner from 0. 002 to 0. 100mg/L, the detection limits of β-1actams antibiotics were 0.1-0. 6μg/kg and the limit of quantitation were 0. 3-1. 8μg/kg. This method is specific, sensitive and suitable for determination of β-1actams antibiot- ics in the milk.

关 键 词：固相萃取 超高效液相色谱-串联质谱 牛奶β-内酰胺类药物 

分 类 号：O657.63[理学—分析化学] TS252.7[理学—化学]