Citation: DUAN Yongsheng, WANG Bingling, AI Lianfeng, GUO Chunhai, GE Shihui, ZHANG Jingwen, XU Niusheng. Determination of six progesterones in milk by on-line cleanup liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2014, 32(6): 647-652. doi: 10.3724/SP.J.1123.2014.01044 shu

Determination of six progesterones in milk by on-line cleanup liquid chromatography-tandem mass spectrometry

1.
1. Hebei Entry-Exit Inspection and Quarantine Bureau, Shijiazhuang 050051, China;

Corresponding author: AI Lianfeng,
Received Date: 27 January 2014
Available Online: 3 April 2014
Fund Project: 国家质检总局科技计划项目(2013IK154,2014IK092). (2013IK154,2014IK092)

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, 17 α-hydroxyprogesterone, medroxyprogesterone, 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 simple, rapid, sensitive and highly selective, and can be applied to simultaneous identification and quantification of the six progesterones in milk.
- on-line cleanup,
- liquid chromatography-tandem mass spectrometry (LC-MS/MS),
- progesterones,
- milk
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沈阳化工大学材料科学与工程学院沈阳 110142