Citation: KE Xing, HUANG Bai-Fen, LÜ Mei-Ling, MO Wei-Min, REN Yi-Ping. Simultaneous Determination of 11 Cholesterol Oxidation Products in Salted Duck Egg Yolk by Enzymolysis-Liquid Chromatography Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2015, 43(12): 1920-1926. doi: 10.11895/j.issn.0253-3820.150514 shu

Simultaneous Determination of 11 Cholesterol Oxidation Products in Salted Duck Egg Yolk by Enzymolysis-Liquid Chromatography Tandem Mass Spectrometry

1.
¹ College of Chemical Engineering;Zhejiang University of Technology, Hangzhou 310014, China;

Corresponding author: HUANG Bai-Fen,
Received Date: 23 June 2015
Available Online: 6 September 2015
Fund Project: 本文系浙江省公益性技术应用研究计划(No.2015C37061)资助 (No.2015C37061)

A method for simultaneous quantification of 11 cholesterol oxidation products(COPs) in yolk of salted duck egg was developed by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) with enzymatic treatment. Firstly, the yolk of salted duck egg was digested by lipase at 37℃, and COPs were extracted by n-hexane and diethyl ether mixture(8:2, V/V). The supernatant was enriched and purified by solid phase extraction of silica. Eleven COPs were separated by UPLC HSS T3 column(100 mm×2.1 mm, 0.3μm) with water and methanol/acetonitrile(1:1, V/V) both containing 0.1% formic acid. All COPs were simultaneously determined by UPLC-MS/MS with multiple reaction monitoring mode(MRM). The d7-7α-OH cholesterol was used as internal standard. The results showed that the linear ranges were 20-1200 ng/mL and 200-3500 ng/mL with correlation coefficient(r ≥ 0.996). The recoveries of three spiking levels were between 79.3% and 104.1%, and relative standard deviations(RSD) were 2.0% and 12.9%. The limit of quantification(LOQ) was 0.08-0.40μg/g. The established method with good repeatability and robust recovery can be applied to quantify the levels of 11 COPs in yolk of salted duck eggs.
- Cholesterol oxidation products,
- Salted duck egg yolk,
- Enzymatic method,
- Liquid chromatography tandem mass spectrometry
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