LC-MS法测定婴儿乳粉中4种激素和氯霉素残留  

Determination of Four Hormones and Chloramphenicol Residues in Infant Formula by LC-MS

作　　者：耿健强[1] 赵丽[1] 潘红艳[1] 邵名媛 孙龙[1] 王浩[1] 

机构地区：[1]国家食品质量安全监督检验中心,北京100094

出　　处：《食品工业》2017年第4期285-289,共5页The Food Industry

摘　　要：建立了高效液相色谱-质谱法测定婴幼儿配方乳粉中壬基酚、双酚A、雌二醇、雌三醇和氯霉素残留的检测方法。样品经0.5%氨水的乙腈超声提取,减压浓缩后复溶于2 m L含2%氨水的甲醇溶液。以MGⅢ-C18色谱柱(4.6 mm×150 mm,1.8μm)分离,流动相为甲醇和10 mmol/L乙酸铵水溶液(0.05%氨水)(梯度洗脱),流速0.35 m L/min。采用多反应监测负离子模式,可以一次性对五种目标化合物进行定性和定量测定。在该优化条件下,检出限为0.1~0.5μg/kg,定量限为0.3~1.5μg/kg,方法回收率为80.1%~106.8%,相对标准偏差(RSD)为3.89%~9.98%。结果表明,该方法前处理简单,灵敏度高,适合于婴幼儿配方乳粉中壬基酚、双酚A、雌二醇、雌三醇和氯霉素残留的同时快速检测。A new liquid chromatography-tandem mass spectrometry （LC-MS/MS） method was established for the simultaneous determination of residues of nonyl phenol, bisphenol A, estmdiol, estriol and chlommphenicol in infant formula. Samples were extracted with acetonilrile containing 0.5% aqueous ammonia. The extract was concentrated by evaporation and redissolved in 2 mL of methanol containing 2% ammonia. The chromatographic separation was carried out on a MG 111-C18 column （4.6 mm×150mm, 1.8 mm） using a mobile phase made up of methanol and 10 mmol/L ammonium acetate aqueous solution （0.05% aqueous ammonia） by gradient elution at a flow rate of 0.35 mL/min. These five compounds could be qualitatively and quantitatively determined by multiple reaction monitoring （MRM） in negative mode simultaneously. The limits of detection and quantification were within 0.1-0.5 mg/kg and 0.3-1.5 mg/kg, respectively. The average spike recoveries of the method ranged from 80.1% to 106.8% with relative standard deviations （RSD） of 3.89%-9.98%. This method was proved to be simple, rapid, sensitive and effective for simultaneously determining five toxic and prohibited substances residues in infant formula.

关 键 词：液相色谱-质谱联用技术 壬基酚 双酚A 雌二醇 雌三醇 氯霉素 

分 类 号：TS252.51[轻工技术与工程—农产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]