色谱Issue(6)：647-652,6.DOI:10.3724/SP.J.1123.2014.01044
在线净化液相色谱-串联质谱法快速测定牛奶中的6种孕激素
Determination of six progesterones in milk by on-line cleanup liquid chromatography-tandem mass spectrometry
摘要
Abstract
A new method using TurboFlow on-line cleanup liquid chromatography combined with tandem mass spectrometry(MS / MS)has been developed for simultaneous determination of six progesterones including 19-norethindrone,17α-hydroxyprogesterone,medroxyprogester-one,megestrol acetate,progesterone and melengestrol acetate in milk. Samples were extracted by acetonitrile. The analytes in extract were on-line purified directly on Cyclone-P purification column where the sample matrices were washed away. Subsequently,the analytes which were eluted from the extraction column onto Phenyl-Hexyl column were separated with a gradient elution,and detected with electrospray ionization mass spectrometry in the positive scan mode using multiple reaction monitoring( MRM). The isotope internal standards were employed for quantification. As a result,the linearities were satisfactory with the correlation coefficients of﹥0. 999 at concentrations ranging from 0. 1 μg / L to 50 μg / L. Based on the repeated analysis of a known blank sample,the limit of quantification(LOQ)is 0. 5 μg / kg. Average recoveries of the analytes fortified at three levels(1,5 and 25 μg / kg)ranged from 90. 8% to 107. 5% ,and the relative standard deviations(RSDs)ranged from 6. 3% to 11. 8% . This proposed method is sim-ple,rapid,sensitive and highly selective,and can be applied to simultaneous identification and quantification of the six progesterones in milk.关键词
在线净化/液相色谱-串联质谱/孕激素/牛奶Key words
on-line cleanup/liquid chromatography-tandem mass spectrometry(LC-MS/MS)/progesterones/milk分类
化学化工引用本文复制引用
段永生,王炳玲,艾连峰,郭春海,葛世辉,张婧雯,徐牛生..在线净化液相色谱-串联质谱法快速测定牛奶中的6种孕激素[J].色谱,2014,(6):647-652,6.基金项目
国家质检总局科技计划项目（2013IK154，2014IK092）． （）
