溶解沉淀-气相色谱-串联质谱法测定塑料玩具中的58种致敏性芳香剂

引用本文: 刘雅慧, 王志娟, 闫正, 张庆, 马强, 白桦, 吕庆. 溶解沉淀-气相色谱-串联质谱法测定塑料玩具中的58种致敏性芳香剂[J]. 分析化学, 2019, 47(1): 129-137. doi: 10.19756/j.issn.0253-3820.181460 shu

Citation: LIU Ya-Hui, WANG Zhi-Juan, YAN Zheng, ZHANG Qing, MA Qiang, BAI Hua, LYU Qing. Determination of 58 Kinds of Fragrance Allergens in Plastic Toys by Dissolution Precipitation-Gas Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2019, 47(1): 129-137. doi: 10.19756/j.issn.0253-3820.181460 shu

溶解沉淀-气相色谱-串联质谱法测定塑料玩具中的58种致敏性芳香剂

刘雅慧 ^1,2, ,
王志娟 ^2, ,
闫正 ^1, ,
张庆 ^2, ,
马强 ^2, ,
白桦 ^2, ,
吕庆 ^2,

1.
河北大学, 化学与环境科学学院, 保定 071002;
2.
中国检验检疫科学研究院, 工业与消费品安全研究所, 北京 100176
基金项目:
本文系国家重点研发计划项目（No.2016YFF0203702）资助

摘要: 基于溶解沉淀-气相色谱-串联质谱（GC-MS/MS）技术，建立了ABS和PVC塑料玩具中58种致敏性芳香剂的同时测定方法。玩具样品在经四氢呋喃溶解、甲醇沉淀后，取上清液过0.22 μm滤膜后检测，通过DB-17MS色谱柱分离，串联质谱多反应监测模式（SRM）测定，外标法定量。对色谱-质谱条件进行优化，通过测定自制阳性样品的回收率，证明溶解沉淀法具有较高的提取率。实验结果表明，GC-MS/MS具有较强的抗基质背景干扰能力，由于存在溶剂效应和基质效应，需要采用空白基质匹配的标准曲线进行定量分析。方法对于不同物质的定量限（LOQ）为0.1~10 mg/kg，在线性范围0.1~600 mg/kg内相关系数（R²）大于0.9926，在ABS和PVC样品中的回收率分别为76.9%-129.6%和70.3%-126.5，相对标准偏差（RSD，n=6）在0.9%-10.2%和1.1%-9.6%之间。最后，对市售的65个玩具样品进行检测，检出的10种芳香剂含量在3.0-46.8 mg/kg之间。本方法简便、快速、准确、灵敏，适用于塑料玩具中58种致敏性芳香剂的检测。

关键词:

English

Determination of 58 Kinds of Fragrance Allergens in Plastic Toys by Dissolution Precipitation-Gas Chromatography-Tandem Mass Spectrometry

1.
College of Chemistry & Environmental Science, Hebei University, Baoding 071002, China;
2.
Institute of Industrial and Consumer Product Safety, Chinese Academy of Inspection and Quarantine, Beijing 100176, China
Received Date: 13 July 2018
Revised Date: 06 October 2018
Fund Project:
This work was supported by the National Key Research and Development Program of China (No.2016YFF0203702).

Abstract: A method was developed for simultaneous determination of 58 kinds of fragrance allergens in acrylonitrile-butadiene-styrene (ABS) and polyvinyl chloride (PVC) plastic toys based on dissolution precipitation-gas chromatography tandem mass spectrometry (GC-MS/MS). Sample was dissolved by tetrahydrofuran, and precipitated by methanol, and then its supernatant was taken through a 0.22-μm filter membrane. After separated by DB-17MS column, the analytes were determined by tandem mass spectrometry in SRM mode, and then quantified by the external standard method. The study optimized the GC-MS parameters for determination of 58 analytes and further proved that the dissolution precipitation method had a high extraction rate by determining the recovery of the homemade positive sample. Its results showed that GC-MS/MS had strong anti-matrix background interference ability. Due to the existence of solvent effect and matrix effect, the matrix matching standard curve method should be used for quantitative analysis. The limits of quantification (LOQs) for different substances were 0.1-10 mg/kg, and the correlation coefficient (R²) was larger than 0.9926 in the linear range of 0.1-600 mg/kg. The recoveries of fragrances in ABS and PVC samples ranged from 76.9% to 129.6% and 70.3% to 126.5%, respectively. The relative standard deviations (RSD, n=6) ranged from 0.9% to 10.2% and 1.1% to 9.6%, respectively. Finally, 65 commercial toys were detected, and the contents of 10 fragrances ranged from 3.0 to 46.8 mg/kg. The method was simple, rapid, accurate, sensitive and low cost, and suitable for the detection of 58 fragrance allergens in plastic toys.

Key words:

Fragrance allergens
/ Dissolution-precipitation
/ Gas chromatography-tandem mass spectrometry
/ Plastic toys

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沈阳化工大学材料科学与工程学院沈阳 110142

溶解沉淀-气相色谱-串联质谱法测定塑料玩具中的58种致敏性芳香剂

English

Determination of 58 Kinds of Fragrance Allergens in Plastic Toys by Dissolution Precipitation-Gas Chromatography-Tandem Mass Spectrometry

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

溶解沉淀-气相色谱-串联质谱法测定塑料玩具中的58种致敏性芳香剂

English

Determination of 58 Kinds of Fragrance Allergens in Plastic Toys by Dissolution Precipitation-Gas 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

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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