【引用本文】 佟玲, 田芹, 杨志鹏, 等. 沉积物中14种典型人工合成麝香加速溶剂萃取-气相色谱-串联质谱快速分析方法研究[J]. 岩矿测试, 2020, 39(4): 587-596. doi: 10.15898/j.cnki.11-2131/td.201906240089
TONG Ling, TIAN Qin, YANG Zhi-peng, et al. Research on the Determination of 14 Synthetic Musks in Sediment Samples by Gas Chromatography-Tandem Mass Spectrometry with Accelerated Solvent Extraction[J]. Rock and Mineral Analysis, 2020, 39(4): 587-596. doi: 10.15898/j.cnki.11-2131/td.201906240089

沉积物中14种典型人工合成麝香加速溶剂萃取-气相色谱-串联质谱快速分析方法研究

国家地质实验测试中心, 北京 100037

收稿日期: 2019-06-24  修回日期: 2019-11-22  接受日期: 2020-05-31

基金项目: 中国地质调查局地质调查项目(DD20190475,DD20190323);中国地质科学院国家地质实验测试中心基本科研业务费项目(CSJ201601)

作者简介: 佟玲, 硕士, 副研究员, 主要从事环境中有机污染物分析与研究。E-mail:winter_tl@sina.com

Research on the Determination of 14 Synthetic Musks in Sediment Samples by Gas Chromatography-Tandem Mass Spectrometry with Accelerated Solvent Extraction

National Research Center for Geoanalysis, Beijing 100037, China

Received Date: 2019-06-24
Revised Date: 2019-11-22
Accepted Date: 2020-05-31

摘要:近年人工合成麝香在环境中污染状况加剧,该类化合物具有潜在致癌和环境激素作用,对人类健康构成了威胁,因此越来越受到科学工作者的重视。水和土壤等环境样品中的人工合成麝香检测技术发展迅速,并朝着快速绿色的方向发展。人工合成麝香在沉积物中的浓度达到了几个到几千个ng/g的水平,但对于沉积物复杂基质中的多种类人工合成麝香,采取同步提取与净化,并快速分析的方法还有待研究。本文建立了沉积物样品中硝基麝香、多环麝香和大环麝香共三类、14种典型人工合成麝香的快速分析方法。通过实验优化了提取溶剂、提取温度、在线净化吸附剂等条件,大大降低了样品的前处理成本。最终确定样品采用加速溶剂萃取,萃取池中依次装入净化吸附剂(0.4g GCB和1.0g SAX)及5.0g沉积物样品,在80℃条件下采用提取溶剂正己烷-丙酮(4:1,V/V)循环提取2次,提取液浓缩后采用气相色谱-三重四极杆串联质谱(GC-MS/MS)进行测定。结果表明:14种目标化合物的线性范围为5~200ng/mL,平均添加回收率为70.6%~121.5%,相对标准偏差(RSD,n=7)为0.97%~19.5%。替代物回收率为72.2%~116.8%,方法检出限为硝基麝香0.10~0.19ng/g,多环麝香0.09~0.14ng/g,大环麝香0.11~1.93ng/g。该方法能够满足复杂基质沉积物样品的分析要求。

关键词: 人工合成麝香, 沉积物, 气相色谱-三重四极杆串联质谱法, 加速溶剂萃取, 复杂基质样品

要点

(1) 沉积物中14种典型人工合成麝香的快速同时分析。

Research on the Determination of 14 Synthetic Musks in Sediment Samples by Gas Chromatography-Tandem Mass Spectrometry with Accelerated Solvent Extraction

ABSTRACT

BACKGROUND:

In recent years, the pollution of synthetic musk in the environment has increased. This kind of material has potential carcinogenic and environmental hormone effects and poses a threat to human health. Therefore, it has attracted increasing attention from scientists. The analytical technology of synthetic musk in environmental samples such as water and soil has developed rapidly. The concentration of synthetic musk in sediments has reached several thousand ng/g, but the methods for the simultaneous extraction and purification and rapid analysis of various types of synthetic musk in complex matrices of sediments are yet to be studied.

OBJECTIVES:

To establish a rapid method for the analysis of 14 typical synthetic musks in sediment samples by accelerated solvent extraction (ASE) combined with gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS).

METHODS:

Accelerated solvent extraction was used for sample preparation. The ASE cell was filled up with sorbent (0.4g GCB combined with 1.0g SAX) and 5.0g sediment samples. The sample was extracted in two cycles with mixed solvents hexane-acetone (V/V, 4:1) at 80℃. After preconcentration, the extracted solution was determined by GC-MS/MS.

RESULTS:

The linear range of this method for fourteen target compounds ranged from 5ng/mL to 200ng/mL. The average spike-added recoveries ranged from 70.6% to 121.5%, the relative standard deviations (RSD, n=7) were 0.97%-19.5%. The recoveries of surrogates were 72.2%-116.8%. The detection limits of the method were 0.10-0.19ng/g for nitro musk, 0.09-0.14ng/g for polycyclic musk, and 0.11-1.93ng/g for macrocyclic musk.

CONCLUSIONS:

This method can satisfy the analysis of musk in sediments with complex matrices.

KEY WORDS: synthetic musks, sediment, gas chromatography-triple quadrupole tandem mass spectrometry, accelerated solvent extraction, complex matrices

HIGHLIGHTS

(1) A method for the rapid and simultaneous analysis of 14 typical synthetic musks in sediments was established.

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沉积物中14种典型人工合成麝香加速溶剂萃取-气相色谱-串联质谱快速分析方法研究

佟玲, 田芹, 杨志鹏, 潘萌