Determination of <italic style="font-style: italic">α</italic>-Chlorotoluene in Cosmetics by Headspace Gas Chromatography－Mass Spectrometry

LIU Hua-chun; LIANG Wen-yao; WANG Ji-cai; XIA Ze-min; XIONG Xiao-ting; PENG Rong-fei; TAN Jian-hua

doi:10.19969/j.fxcsxb.20121001

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Determination of α-Chlorotoluene in Cosmetics by Headspace Gas Chromatography－Mass Spectrometry

Experimental Techniques and Methods | 更新时间：2023-02-13

- Determination of α-Chlorotoluene in Cosmetics by Headspace Gas Chromatography－Mass Spectrometry
- Journal of Instrumental Analysis Vol. 40, Issue 8, Pages: 1230-1234(2021)
- 作者机构：
  
  1.广州市疾病预防控制中心，广东广州 510440
  2.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
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.20121001
  CLC：
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柳华春,梁文耀,王继才等.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(08):1230-1234.

LIU Hua-chun,LIANG Wen-yao,WANG Ji-cai,et al.Determination of α-Chlorotoluene in Cosmetics by Headspace Gas Chromatography－Mass Spectrometry[J].Journal of Instrumental Analysis,2021,40(08):1230-1234.
柳华春,梁文耀,王继才等.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(08):1230-1234. DOI： 10.19969/j.fxcsxb.20121001.

LIU Hua-chun,LIANG Wen-yao,WANG Ji-cai,et al.Determination of α-Chlorotoluene in Cosmetics by Headspace Gas Chromatography－Mass Spectrometry[J].Journal of Instrumental Analysis,2021,40(08):1230-1234. DOI： 10.19969/j.fxcsxb.20121001.

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。

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.

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）

Keywords

α-chlorotoluenecosmeticsbenzalkonium chloridethermal degradationheadspace gas chromatography－mass spectrometry （HS－GC－MS）

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Related Institution

Guangdong Provincial Key Laboratory of Chemical Measurement and Emergency Test Technology，Guangdong Provincial Engineering Research Center for Quality and Safety of Traditional Chinese Medicine，Institute of Analysis，Guangdong Academy of Sciences（China National Analytical Center，），Guangzhou

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Institute of Analysis，Guangdong Academy of Sciences（China National Analytical Center，Guangzhou），Guangdong Provincial Key Laboratory of Chemical Measurement and Emergency Test Technology，Guangdong Provincial Engineering Research Center for Quality and Safety of Traditional Chinese Medicine

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Determination of α-Chlorotoluene in Cosmetics by Headspace Gas Chromatography－Mass Spectrometry

DOI：10.19969/j.fxcsxb.20121001

摘要

Abstract

关键词

Keywords

references