Citation: WEI Xueyuan, SHEN Weijian, YU Keyao, ZHANG Jian, LU Huiyuan, WU Bin, SHEN Chongyu, ZHAO Zengyun, LIU Han, DENG Xiaojun, WANG Suilou. A comparative study of two ionization techniques in gas chromatography-mass spectrometric determination of sterenes in olive oil[J]. Chinese Journal of Chromatography, ;2016, 34(4): 429-435. doi: 10.3724/SP.J.1123.2015.12016 shu

A comparative study of two ionization techniques in gas chromatography-mass spectrometric determination of sterenes in olive oil

WEI Xueyuan ^1,2 ,
SHEN Weijian ² ,
YU Keyao ² ,
ZHANG Jian ² ,
LU Huiyuan ² ,
WU Bin ² ,
SHEN Chongyu ² ,
ZHAO Zengyun ² ,
LIU Han ² ,
DENG Xiaojun ³ ,
WANG Suilou ^1,,

1.
1. College of Pharmacy, China Pharmaceutical University, Nanjing 210009, China;
2.
2. Food Laboratory, Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China;
3.
3. Technical Center for Animal Plant and Food Inspection and Quarantine, Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China

Corresponding author: WANG Suilou,
Received Date: 16 December 2015

Fund Project: 国家质检总局科技计划项目(2015IK141) (2015IK141)江苏省"333工程"项目(BRA2014330) (BRA2014330)上海长三角科技合作项目(15395810100). (15395810100)

The gas chromatography-mass spectrometric (GC-MS) method with two different ionization techniques, electron impact (EI) and positive chemical ionization (PCI), have been developed for the simultaneous determination of three sterenes in olive oil. The olive oil sample was dissolved in petroleum ether, followed by cleanup on a silica gel column and finally analyzed by GC-EI/MS and GC-PCI/MS in selected ion monitoring mode. The quantitation was performed by internal standard calibration with cholesta-3, 5-diene as internal standard. These two methods were compared in terms of linearity, accuracy, precision and sensitivity. Good linearities were obtained with correlation coefficients (r) higher than 0.999 for campesta-3, 5-diene in the range of 0.024 to 0.48 mg/L, stigmasta-3, 5, 22-triene in the range of 0.02 to 0.50 mg/L and stigmasta-3, 5-diene in the range of 0.03 to 0.75 mg/L. The accuracy test was carried out at three spiked levels in extra virgin olive oil. The average recoveries ranged from 88.7% to 99.5% (EI) and 87.1% to 109.2% (PCI), with relative standard deviations (RSDs, n=6) not higher than 8.3%. Limits of quantification (LOQs, S/N=10) were 0.03 mg/kg (EI) and 0.03-0.10 mg/kg (PCI). Comparative analysis showed a large number of fragment ions could be obtained in EI mode while quasi-molecular ions or other adduct molecular ions were the most abundant ion formed in the PCI mode. Besides, PCI has a better selectivity than EI when applied to real samples. In conclusion, these two ionization techniques are complementary and alternative in the routine analysis of sterenes in olive oil.
- gas chromatography-mass spectrometry (GC-MS),
- sterenes,
- electron impact ionization (EI),
- positive chemical ionization (PCI)
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