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气相色谱-质谱法测定儿童餐具中芳香胺迁移量
王国军1,黄丹2,陈莉2,洪瑜隆1,林铿1,颜林平1
1.台州方圆质检有限公司,浙江 台州 318000;2.台州市产品质量安全检测研究院,浙江 台州 318000
摘要:
目的 建立气相色谱-质谱法测定新型儿童餐具中23种初级芳香胺(Primary aromatic amines,简称PPAs)在模拟唾液中的迁移量的分析方法。方法 试样经模拟唾液振荡提取,二氯甲烷萃取后浓缩,甲醇定容后经气质联用仪分析,外标法定量。结果 该法在0.001~0.15 mg/dm2范围内具有良好的线性关系,相关系数(r)均大于0.998。方法的检出限为0.0001~0.0005 mg/dm2,加标回收率为85%~108%,相对标准偏差(RSD)为1.5%~8.7%,可满足测试要求。按照建立的方法,对10个实际样品进行测定,其中有9个样品检出了芳香胺。结论 该方法操作简便,灵敏度高,结果准确可靠,重现性好,贴近样品实际使用状态,能够满足新型儿童餐具中芳香胺迁移量的测定,并可为儿童餐具相关标准的制定及安全性评价提供数据支持和方法指导。
关键词:  儿童餐具  芳香胺  模拟唾液  气相色谱-质谱法
DOI:10.19554/j.cnki.1001-3563.2020.21.020
分类号:TB487
基金项目:浙江省质量技术监督局计划(20140274);台州市211人才工程项目
Determination of Migration of Aromatic Amines in Children's Tableware by Gas Chromatography-Mass Spectrometry
WANG Guo-jun1, HUANG Dan2, CHEN Li2, HONG Yu-long1, LIN Keng1, YAN Lin-ping1
(1.Taizhou Fangyuan Test Co., Ltd., Taizhou 318000, China;2.Taizhou Institute of Product Quality and Safety Inspection, Taizhou 318000, China)
Abstract:
The work aims to establish a gas chromatography-mass spectrometry method to determine the migration of 23 primary aromatic amines (PPAs) of new children's tableware in simulated saliva. The sample was extracted by simulated saliva shaking and the dichloromethane was extracted and then concentrated. The methanol with volume metered was analyzed by gas chromatography-mass spectrometry and quantified by external standard method. The method had a good linear relationship in the range of 0.001-0.15 mg/dm2, and the correlation coefficients (r) were all greater than 0.998. The detection limit of the method was 0.0001-0.0005 mg/dm2, the spiked recovery was 85%-108%, and the RSD was 1.5%-8.7%, which met the test requirements. According to the method established above, 10 actual samples were measured, and 9 of them had aromatic amines.The method is simple and accurate, with high sensitivity and good reproducibility and can be close to the actual use state of sample, so it can meet the determination of aromatic amine migration in new children's tableware, and provide data support and method guidance for the development of safety standards and evaluation of children's tableware.
Key words:  children's tableware  aromatic amine  simulant saliva  gas chromatography-mass spectrometry method

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