分析化学2011，Vol.39Issue(9)：1323-1328,6.DOI:10.3724/SP.J.1096.2011.01323
超高效液相色谱-四极杆飞行时间串联质谱法同时分析奶粉中9种雌激素
Simultaneous Analysis of Nine Estrogens in Milk Powder with Ultra Performance Liquid Chromatography Coupled Quadrupole Time-of-Flight Mass Spectrometry
摘要
Abstract
A rapid, sensitive and specific method has been developed for the simultaneous analysis of 9 estrogens including estradiol,β-estradiol, α-estradiol, equilin, 17α-ethinylestradiol, estrone, dieth-ylstilbestrol, dienestrol and hexestrol using ultra-performance liquid chromatography coupled quadru-pole time-of-flight mass spectrometry(UPLC-Q-TOF-MS)with electrospray ionization (ESI) in negative mode. The milk powder was dissolved in water, the estrogens were extracted with acetonitrile using ultra-sonication and the lipids in extract solution were removed by n-hexane liquid-liquid extraction. Then the estrogens were purified by the NH2 solid phase extraction cartridge, separated on a Waters ACQUITY UPLC HSS T3 column (100 mm×2. 1 mm×1. 8 μm) and analyzed qualitatively and quantitatively by UPLC-Q-TOF in MS and MSe mode. The overall analysis time of the method was 13 min and the linear range was 0. 001 to 0. 5 mg/L. The limits of detection (LOD) for the compounds were from 0. 11 to 0. 30 μg/kg and the limits of quantification (LOQ) were in the range of 0. 37-1. 0 μg/kg. The mass errors between theoretical and experimental masses obtained for deproto-nated molecules of 9 estrogens and internal standard (β-estradiol-d3) were between - 1. 0 and 0. 9 mDa. At the spiked levels of 1, 2, 10, 100 ug/kg, the average recoveries were 61% -137% with the relative standard deviations of 1. 0% -22. 6%. The results showed that this method is suitable to the multi-residue detection of estrogens in milk powder. It has been applied to the analysis of seven real milk powder samples, and the target estrogens were not found.关键词
超高效液相色谱-四极杆飞行时间串联质谱/QuEchERS方法/雌激素/奶粉Key words
Ultra performance liquid chromatography coupled quadrupole time-of-flight mass spec- trometry/ Estrogens/ Milk powder引用本文复制引用
王和兴,周颖,姜庆五..超高效液相色谱-四极杆飞行时间串联质谱法同时分析奶粉中9种雌激素[J].分析化学,2011,39(9):1323-1328,6.基金项目
本文系国家“十一五”科技支撑计划(No.2006BAI19B02)和复旦大学09年青年基金(No.EYF201023)资助 （No.2006BAI19B02）
