同位素内标UPLC_MS_MS法测定婴儿配方奶粉中性激素苯甲酸雌二醇残留指南.pdfVIP

350 2009, Vol. 30, No. 20 食品科学 ※分析检测 同位素内标UPLC -MS/MS法测定婴儿 配方奶粉中性激素苯甲酸雌二醇残留 1 1 2 王全林 ，张爱芝 ，陈立仁 (1.宁波市产品质量监督检验研究院，浙江 宁波 3 1504 1；2 .中国科学院兰州化学物理研究所，甘肃兰州 730000) 摘 要：建立测定婴儿配方奶粉中性激素苯甲酸雌二醇的超高效液相色谱- 串联质谱方法。样品前处理采用酶解、 甲醇提取，经LC-C18 和LC-NH2 基固相萃取柱净化。苯甲酸雌二醇由超高效液相色谱- 串联质谱(UPLC-MS/MS)分 + 离、在正离子电离模式(ESI )及多反应监测模式(MRM)下，以氘代诺龙-d3 为内标进行定量检测。方法对婴儿配方 奶粉中苯甲酸雌二醇的检出限(LOD)0.39 μg/kg ，定量限(LOQ)为0.95 μg/kg 。在4 μg/kg 和10 μg/kg 两个加标水平下， 婴儿配方奶粉中苯甲酸雌二醇的回收率在76.5%～86.3% 的范围内，相对标准偏差在9.7%～15.2% 范围内。 关键词：婴儿配方奶粉；U P L C -M S/ M S ；同位素内标法；性激素；苯甲酸雌二醇残留 UPLC-MS/MS Isotopic Internal Standard Determination of Estradiol Benzoate Residues in Infant Formula Milk Powder 1 1 2 WANG Quan-lin ，ZHAN G Ai-zhi ，CHEN Li-ren ( 1. Ningbo Academy of Product Quality Supervision and Inspection, Ningbo 3 1504 1, China； 2. Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, China) Abstract ：UPLC-MS/MS, a highly specific and sen sitive method, was successfully developed for determining estradiol benzoate residues in infant formula milk powder. Sample preparation was involved in enzymatic digestion , extraction with methanol and clean-up by solid-phase extraction (SPE) combining C18 and NH2 columns. Estradiol benzoate was detected by ultra- performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) in a positive ionization mode