Citation: QIAN Ye, ZHANG Yawei, WANG Zhen, YIN Jing, PENG Zengqi, ZHOU Guanghong. Determination of five cholesterol oxidation products in marinated pig feet and hocks by gas chromatography-mass spectrometry[J]. Chinese Journal of Chromatography, ;2019, 37(5): 539-546. doi: 10.3724/SP.J.1123.2018.11020 shu

Determination of five cholesterol oxidation products in marinated pig feet and hocks by gas chromatography-mass spectrometry

QIAN Ye ^1,2, ,
ZHANG Yawei ^1,2 ,
WANG Zhen ^1,2 ,
YIN Jing ^1,2 ,
PENG Zengqi ^1,2 ,
ZHOU Guanghong ^1,2

1.
College of Food Science and Technology, Nanjing Agricultural University, Nanjing 210095, China;
2.
Synergetic Innovation Center of Food Safety and Nutrition, Nanjing 210095, China

Received Date: 13 November 2018

Fund Project: National Key R & D Program During the Thirteenth Five-Year Plan Period (No. 2018YFD0502306).

An analytical method was developed for the simultaneous determination of five cholesterol oxidation products (COPs) in marinated pig feet and hocks by gas chromatography-mass spectrometry (GC-MS). The five COPs were 7 β -hydroxycholesterol, cholesterol-5 α,6 α -epoxide, 3 β,5 α,6 β -trihydroxycholestane, 25-hydroxycholesterol and 7-ketocholesterol. The sample was extracted with methanol-chloroform (1:2, v/v) and purified by solid phase extraction. Subsequently, the sample was collected for derivatization by N,O-bis(trimethylsilyl)acetamide-trimethyl chlorosilane-1-trimethylsilyllimidazole (3:2:3, v/v/v) (Sylon BTZ). The column temperature was properly programmed, and the selected ion monitoring (SIM) mode was used for the determination of COPs. Under optimum conditions, the five COPs were well separated within 22 min with good separation. The linear range of the five COPs met the requirement of determination, and the average recoveries of the five COPs spiked in the pork samples at three levels were 61.16%-96.96% with relative standard deviations (RSDs) no more than 7.80% (n=3). The limits of detection (LODs) and limits of quantification (LOQs) were in the range of 0.02-47.07 ng/g and 0.06-156.90 ng/g, respectively. This method has a wide line arrange and high sensitivity, and has been successfully applied to the analysis of COPs in actual samples.
- gas chromatography-mass spectrometry (GC-MS),
- solid phase extraction (SPE),
- cholesterol oxidation products (COPs),
- marinated pig feet,
- marinated pig hock
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