超声萃取-高效液相色谱-串联质谱法测定大气颗粒物中甾醇类化合物

引用本文: 赵起越, 赵红帅, 刘保献, 王焱, 骆昉. 超声萃取-高效液相色谱-串联质谱法测定大气颗粒物中甾醇类化合物[J]. 分析化学, 2016, 44(5): 740-746. doi: 10.11895/j.issn.0253-3820.150783 shu

Citation: ZHAO Qi-Yue, ZHAO Hong-Shuai, LIU Bao-Xian, WANG Yan, LUO Fang. Determination of 4 Sterols in Atmospheric Particles by Ultrasonic Extraction Coupled with High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2016, 44(5): 740-746. doi: 10.11895/j.issn.0253-3820.150783 shu

超声萃取-高效液相色谱-串联质谱法测定大气颗粒物中甾醇类化合物

赵起越 ^1, ,
赵红帅 ^1, ,
刘保献 ^1, ,
王焱 ^1, ,
骆昉 ^2,

1.
北京市环境保护监测中心, 北京 100048;
2.
沃特世科技(上海)有限公司, 上海 201206
基金项目:
本文系北京市优秀人才培养资助青年骨干个人项目(No.2014000021733G210)资助

摘要: 采用超声萃取与液相色谱-串联质谱联用,建立了快速测定大气颗粒物中甾醇类化合物的方法。甾醇类化合物用甲醇超声萃取,浓缩后使用液相色谱-串联质谱分析。采用Waters公司Atlantis C₁₈色谱柱(100 mm×2.1 mm,3μm),以乙腈和水混合流动相梯度洗脱,实现了胆甾醇、豆甾醇、菜油甾醇及β-谷甾醇的分离。并在APCI-MS/MS MRM模式下定量检测。在选取的实验条件下,方法回收率在80.3%~97.7%之间,检出限0.015 ng/m³,相对标准偏差小于15%,日内及日间测定精密度小于20%。本方法具有较好的准确性及精密度,实际样品的测试结果表明,方法可以满足大气颗粒物中甾醇类化合物的定量分析要求。

关键词:

English

Determination of 4 Sterols in Atmospheric Particles by Ultrasonic Extraction Coupled with High Performance Liquid Chromatography-Tandem Mass Spectrometry

1.
Beijing Municipal Environmental Monitoring Center, Beijing 100048, China;
2.
Waters Sci. & Technol. Co. Ltd. (Shanghai), Shanghai 201206, China
Received Date: 08 October 2015
Revised Date: 17 December 2015

Abstract: A rapid analytical method was developed for the determination of 4 sterols in atmospheric particles by ultrasonic extraction coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). After extraction by methanol and enrichment, sterols were separated on an Atlantis C₁₈ column (100 mm×2.1 mm, 3 μm) with acetonitrile and water served as mobile phase in gradient elution, then determined by HPLC-MS/MS using atmospheric pressure chemical positive ionization (APCI⁺) and multiple reaction monitoring (MRM). Parameters of chromatography and mass spectrometry, as well as conditions of ultrasonic extraction were optimized. The developed method provided good linearity (R>0.99) and high recoveries (80.3%-97.7%) for 4 sterols. Low detection limits were obtained as 0.015 ng/m³, with RSD less than 15% (n=6). Comparing with GC/MS, this method was more rapid, sensitive and economical because the derivation was eliminated from the procedure, thus saving a lot of resources. Samples of atmospheric particles were detected using this method, and the results indicated that this method could meet the requirements for quantitative analysis of sterols in atmosphere.

Key words:

Ultrasonic extraction
/ High performance liquid chromatography-tandem mass spectrometry
/ Atmospheric particles
/ Sterol

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沈阳化工大学材料科学与工程学院沈阳 110142

超声萃取-高效液相色谱-串联质谱法测定大气颗粒物中甾醇类化合物

English

Determination of 4 Sterols in Atmospheric Particles by Ultrasonic Extraction Coupled with High Performance Liquid Chromatography-Tandem Mass Spectrometry

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中国化学会秘书处

超声萃取-高效液相色谱-串联质谱法测定大气颗粒物中甾醇类化合物

English

Determination of 4 Sterols in Atmospheric Particles by Ultrasonic Extraction Coupled with High Performance Liquid Chromatography-Tandem Mass Spectrometry

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

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CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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通讯作者: 陈斌, bchen63@163.com

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