多次溶剂萃取-气相色谱/串联质谱法测定热熔胶中的多环芳烃

引用本文: 司晓喜, 朱瑞芝, 张凤梅, 刘春波, 徐艳群, 李中昌, 何沛, 刘志华. 多次溶剂萃取-气相色谱/串联质谱法测定热熔胶中的多环芳烃[J]. 分析化学, 2016, 44(3): 430-436. doi: 10.11895/j.issn.0253-3820.150739 shu

Citation: SI Xiao-Xi, ZHU Rui-Zhi, ZHANG Feng-Mei, LIU Chun-Bo, XU Yan-Qun, LI Zhong-Chang, He Pei, LIU Zhi-Hua. Determination of Polycyclic Aromatic Hydrocarbons in Hot Melt Adhesive by Multiple Solvent Extraction Coupled with Gas Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2016, 44(3): 430-436. doi: 10.11895/j.issn.0253-3820.150739 shu

多次溶剂萃取-气相色谱/串联质谱法测定热熔胶中的多环芳烃

1.
云南省烟草化学重点实验室, 云南中烟工业有限责任公司技术中心, 昆明 650231

通讯作者: 刘志华

基金项目:
本文系中国烟草总公司标准项目(No.2013QB015) (No.2013QB015)

云南中烟工业有限责任公司科技开发项目(No.2015JC06)资助 (No.2015JC06)

摘要: 建立了热熔胶中16 种多环芳烃(PAHs)的多次溶剂萃取-气相色谱/串联质谱测定方法。详细研究了样品的萃取条件、净化条件和气相色谱/串联质谱测定条件,并与气相色谱-质谱法进行了对比。样品以10 mL正己烷为萃取溶剂,于60℃超声萃取20 min,萃取液依次经冷冻后离心、二甲基亚砜萃取2次、正己烷反萃取2次进行净化,得到的净化液以气相色谱/串联质谱法多反应监测(MRM)模式进行检测。本方法的线性相关系数(R²)均大于0.9969,检出限为1.0-10 μg/kg,精密度小于6.3%,16 种PAHs的加标回收率为80.4%-117.6%。考察了串联质谱检测的基质效应,发现基质效应不明显。本方法检出限优于气相色谱-质谱法(23-94 μg/kg),并能增加定性和定量分析的准确性。本方法灵敏、准确可靠,满足热熔胶中PAHs测试要求。

关键词:

English

Determination of Polycyclic Aromatic Hydrocarbons in Hot Melt Adhesive by Multiple Solvent Extraction Coupled with Gas Chromatography-Tandem Mass Spectrometry

1.
Key Laboratory of Tobacco Chemistry, R&D Center of China tobacco Yunnan Industrial Co., Ltd., Kunming 650231, China

Corresponding author: 刘志华

Received Date: 17 September 2015
Fund Project:
本文系中国烟草总公司标准项目(No.2013QB015)

云南中烟工业有限责任公司科技开发项目(No.2015JC06)资助

Abstract: A method for multiple solvent extraction coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS) was established for the simultaneous determination of 16 polycyclic aromatic hydrocarbons (PAHs) in hot melt adhesive. The extraction conditions, purification conditions, chromatogphic conditions and tandem MS conditions of analysis were critically examined. The results were also compared with those obtained by gas chromatography-mass spectrometry (GC-MS). The sample was extracted by ultrasonic extraction with n-hexane as solvent at 60℃. Then, the extract was purified by centrifugation after freezing treatment, twice extraction with dimethyl sulfoxide, twice re-extraction with n-hexane in turn. The purified extract was determined by gas chromatography-tandem mass spectrometry under multiple reaction monitoring (MRM) mode. The linear correlation coefficients were above 0.9969, the limits of detection (LOD) ranged from 1.0 μg/kg to 10 μg/kg, the relative standard deviations (RSDs) were below 6.3%, and the recoveries ranged from 80.4% to 117.6% at three spiked levels. The matrix effects of tandem MS were studied, but there was no significance. Compared with GC-MS methods, the established method outperformed the GC-MS methods in LOD, which ranged from 23 μg/kg to 94 μg/kg for GC-MS, and could greatly enhance the accuracy of the qualitative and quantitative analysis of PAHs. The results indicated that the method was sensitive, accurate and reproducible, and suitable for the simultaneous determination of 16 PAHs in hot melt adhesive.

Key words:

Polycyclic aromatic hydrocarbons
/ Solvent extraction
/ Gas chromatography-tandem mass spectrometry
/ Hot melt adhesive

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

多次溶剂萃取-气相色谱/串联质谱法测定热熔胶中的多环芳烃

通讯作者: 刘志华

English

Determination of Polycyclic Aromatic Hydrocarbons in Hot Melt Adhesive by Multiple Solvent Extraction Coupled with Gas Chromatography-Tandem Mass Spectrometry

Corresponding author: 刘志华

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

多次溶剂萃取-气相色谱/串联质谱法测定热熔胶中的多环芳烃

通讯作者: 刘志华

English

Determination of Polycyclic Aromatic Hydrocarbons in Hot Melt Adhesive by Multiple Solvent Extraction Coupled with Gas Chromatography-Tandem Mass Spectrometry

Corresponding author: 刘志华

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

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

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

中国化学会秘书处

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs