食品科学2018，Vol.39Issue(8)：314-321,8.DOI:10.7506/spkx1002-6630-201808049
QuEChERS-UPLC-MS/MS同时测定牛奶和奶粉中42种类固醇激素
Simultaneous Determination of 42 Steroid Hormones in Milk and Milk Powder by QuEChERS Combined with UPLC-MS/MS
陈晓鹏 1顾采琴 2綦艳 2张施敬1
作者信息
- 1. 广东产品质量监督检验研究院,广东 佛山 528300
- 2. 广州大学化学化工学院食品系,广东 广州 510006
- 折叠
摘要
Abstract
A modified quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction method was developed for the simultaneous determination of 42 steroid hormones in milk and milk powder by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Sample pretreatment was studied and the detection conditions were optimized to obtain a rapid and accurate method. The steroid hormones from samples were extracted with 0.1% formic acid in acetonitrile followed by a salting-out step with anhydrous MgSO4and NaCl. After centrifugation, the supernatant was cleaned up with 50 mg of octadecylsilane (C18), 100 mg of primary secondary amine (PSA), and 300 mg of aluminum oxide (Al2O3-N) and re-dissolved with 40% formic acid acetonitrile. The separation was performed on a Waters ACQUITY UPLC? BEH C18column (2.1 mm × 100 mm, 1.7 μm) with gradient elution using acetonitrile and water containing 0.1% formic acid as the mobile phase. The electrospray ionization mass spectrometry was operated in the positive mode using multiple reaction monitoring (MRM). The target compounds were quantified by the matrix-matched external standard method. Under the optimal conditions, the calibration curves of all the analytes were linear in the concentration range of 0.5-500 μg/L with correlation coefficients larger than 0.99. The limits of quantitation (LOQs) ranged from 0.06-1.5 μg/kg. The average recoveries for milk and milk powder at three spiked levels ranged from 70.3%-118.1% with relative standard deviations (RSDs) of 0.6%-14.7%. The method due to its simplicity, rapidity, high accuracy and high precision was suitable for the simultaneous detection of 42 steroid hormones in milk and milk powder.关键词
分散固相萃取QuEChERS/超高效液相色谱-串联质谱/牛奶/奶粉/类固醇激素Key words
QuEChERS/ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)/milk/milk powder/steroid hormones分类
轻工纺织引用本文复制引用
陈晓鹏,顾采琴,綦艳,张施敬..QuEChERS-UPLC-MS/MS同时测定牛奶和奶粉中42种类固醇激素[J].食品科学,2018,39(8):314-321,8.
