Citation: WANG Yu-Ning, CHEN Jun-Hui, HE Xiu-Ping, WANG Jiu-Ming, XIN Ming, WANG Bao-Dong, WANG Xiao-Ru. Determination of Phytosterols in Marine Sediment by Liquid Chromatography-Dopant-assisted Atmospheric Pressure Photoionization Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2021, 49(2): 282-291. doi: 10.19756/j.issn.0253-3820.201595 shu

Determination of Phytosterols in Marine Sediment by Liquid Chromatography-Dopant-assisted Atmospheric Pressure Photoionization Mass Spectrometry

WANG Yu-Ning ¹ ,
CHEN Jun-Hui ^1,2,3,, ,
HE Xiu-Ping ^1,2 ,
WANG Jiu-Ming ¹ ,
XIN Ming ¹ ,
WANG Bao-Dong ^1,2 ,
WANG Xiao-Ru ^1,3

1.
Marine Bioresource and Environment Research Center, Key Laboratory of Marine Eco-Environmental Science and Technology, First Institute of Oceanography, Ministry of Natural Resources, Qingdao 266061, China;
2.
Laboratory for Marine Ecology and Environmental Science, Qingdao National Laboratory for Marine Science and Technology, Qingdao 266071, China;
3.
Xiamen Huaxia University, Xiamen 361024, China

Corresponding author: CHEN Jun-Hui, jhchen@fio.org.cn
Received Date: 10 October 2020
Revised Date: 2 December 2020

Fund Project: Supported by the National Natural Science Foundation of China-Shandong Joint Fund for Marine Ecology and Environmental Sciences (Nos.U1706217, U1606404).

Phytosterol biomarkers in marine sediments are often used to indicate the source of the sedimentary organics in the ocean, and to reflect the evolution of marine ecosystem and environment. In this study, a novel method for simultaneous determination of common phytosterols in marine sediments by non-aqueous reversed-phase liquid chromatography-atmospheric pressure photoionization mass spectrometry (LC-APPI-MS) was established. First, the APPI-MS characteristics of phytosterols were clarified. Under the positive APPI mode, phytosterols tended to produce stable characteristic ion peaks such as[M+H-H₂O]⁺,[M+H-H₂]⁺ and[M+H-2H₂]⁺. In the process of APPI-MS², abundant fragment ion peaks were produced mainly through i-heterolysis. Second, LC-APPI-MS conditions were optimized, and a reversed-phase C₁₈ column was used to separate phytosterols with pure methanol as mobile phase and toluene as APPI ionization dopant, which could realize high sensitivity of detection for phytosterols in sediments. Furthermore, the method showed strong matrix interference resistance ability, good linear relationship (R² ≥ 0.9990), high recovery rate (86.4%-94.9%) and good repeatability (RSDs ≤ 8.3%). Finally, the proposed method was applied to detect common phytosterols in the surface sediment of Laizhou Bay in China, and several sterols, such as brassicasterol, fucosterol and sitosterol, etc., were detected in every sediment sample. The total concentration of sterols was 4.21-12.91 μg/g, among which the concentration of sitosterol was the highest. To sum up, the developed LC-APPI-MS method was a powerful tool for determination of common phytosterols in marine sediments, with easy-operation and high sensitivity.
- Atmospheric pressure photoionization,
- Dopant,
- Marine sediment,
- Phytosterols,
- Laizhou Bay
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沈阳化工大学材料科学与工程学院沈阳 110142

Determination of Phytosterols in Marine Sediment by Liquid Chromatography-Dopant-assisted Atmospheric Pressure Photoionization Mass Spectrometry

南开大学师唯/华北电力大学（保定）刘景维：二维配位聚合物中有序的亲锂冠醚位点用于无枝晶锂沉积

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通讯作者: 陈斌, bchen63@163.com