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顶空气相色谱-质谱联用法测定化妆品中α-氯甲苯
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作者单位
柳华春, 梁文耀,王继才,夏泽敏,熊小婷,彭荣飞,谭建华 1. 广州市疾病预防控制中心广东 广州 5104402. 广州质量监督检测研究院国家化妆品质量监督检验中心 (广州)广东 广州 511447 
基金项目:广州市卫生健康科技项目(20191A010043)
中文摘要:该文建立了一种适用于含苯扎氯铵的化妆品中α-氯甲苯的测定方法。首先通过气相色谱-质谱联用 法(GC-MS)剖析苯扎氯铵热分解产物的成分,确证了苯扎氯铵类化合物在气相进样口会分解产生α-氯甲苯。 采用气液平衡的顶空进样方式,并通过优化顶空进样参数、色谱分离和质谱测定条件,建立了一种化妆品中 α-氯甲苯的新型分析方法。选择顶空平衡温度和时间分别为80 ℃和30 min,样品于顶空瓶中用8 mL水和1. 0 g 氯化钠分散,以 HP-INNOWax 色谱柱(60 m × 0. 25 mm × 0. 25 μm)分离,采用选择离子监测模式(SIM)检 测,外标法定量。结果显示:α-氯甲苯在0. 01~5. 00 μg/mL质量浓度范围内与对应的峰面积呈良好的线性关 系(r = 0. 999),方法检出限和定量下限分别为0. 02 μg/g和0. 05 μg/g,加标回收率为91. 3%~98. 8%,相对标 准偏差(RSD)为1. 5%~4. 9%。该方法操作简便,快速,灵敏度高,专一性好,能有效解决现有方法假阳性干 扰的问题,适用于各种化妆品中α-氯甲苯的准确测定。
中文关键词:α-氯甲苯  化妆品  苯扎氯铵  热降解  顶空气相色谱-质谱联用法(HS-GC-MS)
 
Determination of α-Chlorotoluene in Cos? metics by Headspace Gas Chromatogra? phy-Mass Spectrometry
Abstract:A method was developed for the determination of α-chlorotoluene in cosmetics containing benzalkonium chloride. Firstly, the thermal decomposition products of benzalkonium chloride was analyzed by gas chromatography-mass spectrometry(GC-MS). A phenomenon was confirmed that benzalkonium chloride and similar compounds will decompose into α-chlorotoluene at the inlet of GC-MS. Then, a new analytical method for α-chlorotoluene in cosmetics was developed by a headspace injection mode of gas-liquid equilibrium. The headspace sampling parameters, chromatographic separation and mass spectrometry conditions were optimized. The equilibrium temperature and time for headspace sampler were set at 80 ℃ and 30 min, respectively. The sample was dissolved with 8 mL water and 1.0 g sodium chloride in headspace bottle. The analytes were separated on an HP-INNOWax column(60 m × 0.25 mm × 0.25 μm), then detected in selectedion monitoring mode and quantified by external standard method. Results showed that the standard curves for α-chlorotoluene were linear over the concentration range of 0.01-5.00 μg/mL with linear correlation coefficients(r) of 0.999. The detection limits and quantification limits of the method were 0.02 μg/g and 0.05 μg/g, respectively. The spiked recoveries ranged from 91.3% to 98.8% with relative standard deviations(RSDs) of 1.5%-4.9%. The method is simple, rapid, high sensitive and specific, and it is suitable for the determination of α-chlorotoluene in cosmetics.
Key Words:α-chlorotoluene  ?cosmetics  ?benzalkonium chloride  ?thermal degradation  ?headspace gas chromatography-mass spectrometry (HS-GC-MS)
引用本文:柳华春, 梁文耀,王继才,夏泽敏,熊小婷,彭荣飞,谭建华.顶空气相色谱-质谱联用法测定化妆品中α-氯甲苯[J].分析测试学报,2021,40(8):1230-1234.
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