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

doi:10.7506/spkx1002-6300-200920078

食品科学 ›› 2009, Vol. 30 ›› Issue (20 ): 350-355.doi: 10.7506/spkx1002-6300-200920078

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

王全林¹，张爱芝¹，陈立仁²

1.宁波市产品质量监督检验研究院 2.中国科学院兰州化学物理研究所

收稿日期:2009-06-30 出版日期:2009-10-15 发布日期:2010-12-29
通讯作者: 王全林
基金资助:
浙江省质检系统重大科研计划项目(20070106)

UPLC-MS/MS Isotopic Internal Standard Determination of Estradiol Benzoate Residues in Infant Formula Milk Powder

WANG Quan-lin1，ZHANG Ai-zhi1，CHEN Li-ren2

1. Ningbo Academy of Product Quality Supervision and Inspection, Ningbo 315041, China；
2. Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, China

Received:2009-06-30 Online:2009-10-15 Published:2010-12-29
Contact: WANG Quan-lin

摘要/Abstract

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)0.39μg/kg，定量限(LOQ)为0.95μg/kg。在4μg/kg和10μg/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, UPLC-MS/MS, 同位素内标法, 性激素, 苯甲酸雌二醇残留

Abstract:

UPLC-MS/MS, a highly specific and sensitive 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 and a multiple reaction monitoring (MRM) mode via electrospray ionization (ESI) source and quantitatively determined using nandrolone-d3 as an internal standard. The limit of detection (LOD) and limit of quantification (LOQ) using this method were 0.39 and 0.95 μg/kg for infant formula milk powder respectively. The recovery rates of estradiol benzoate spiked in infant formula milk powder at levels of 4 and 10 μg/kg were ranged from 76.5% to 86.3% with a relative standard deviations in the range of 9.7%－15.2%.

Key words: infant formula milk powder, UPLC-MS/MS, isotopic internal standard method, hormone, estradiol benzoate

中图分类号:

O657.63

王全林1，张爱芝1，陈立仁2. 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[J]. 食品科学, 2009, 30(20 ): 350-355.

WANG Quan-lin1，ZHANG Ai-zhi1，CHEN Li-ren2. UPLC-MS/MS Isotopic Internal Standard Determination of Estradiol Benzoate Residues in Infant Formula Milk Powder[J]. FOOD SCIENCE, 2009, 30(20 ): 350-355.

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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

UPLC-MS/MS Isotopic Internal Standard Determination of Estradiol Benzoate Residues in Infant Formula Milk Powder

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