Rapid Screening of 297 Risk Substances in Cream Cosmetics Using QuEChERS Combined with HPLC-Q-TOF MS

WANG Lu; ZENG Guang-feng; HOU Ying-ye; DONG Jie; CAI Cui-ling; XIAO Ke-yin; ZHANG Xian-chen; LI Jia-yi; XIE Jian-jun

doi:10.19969/j.fxcsxb.23032501

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Rapid Screening of 297 Risk Substances in Cream Cosmetics Using QuEChERS Combined with HPLC-Q-TOF MS

Scientific Papers | 更新时间：2023-09-19

- Rapid Screening of 297 Risk Substances in Cream Cosmetics Using QuEChERS Combined with HPLC-Q-TOF MS
- Journal of Instrumental Analysis Vol. 42, Issue 9, Pages: 1085-1095(2023)
- 作者机构：
  
  1.广州海关技术中心，广东广州 510623
  2.国家级进出口食品质量安全风险验证评价实验室（化妆品），广东广州 510623
  3.中山海关技术中心，广东中山 528400
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.23032501
  CLC：
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王璐,曾广丰,侯颖烨等.QuEChERS结合HPLC-Q-TOF MS快速筛查霜膏类化妆品中297种风险物质[J].分析测试学报,2023,42(09):1085-1095.

WANG Lu,ZENG Guang-feng,HOU Ying-ye,et al.Rapid Screening of 297 Risk Substances in Cream Cosmetics Using QuEChERS Combined with HPLC-Q-TOF MS[J].Journal of Instrumental Analysis,2023,42(09):1085-1095.
王璐,曾广丰,侯颖烨等.QuEChERS结合HPLC-Q-TOF MS快速筛查霜膏类化妆品中297种风险物质[J].分析测试学报,2023,42(09):1085-1095. DOI： 10.19969/j.fxcsxb.23032501.

WANG Lu,ZENG Guang-feng,HOU Ying-ye,et al.Rapid Screening of 297 Risk Substances in Cream Cosmetics Using QuEChERS Combined with HPLC-Q-TOF MS[J].Journal of Instrumental Analysis,2023,42(09):1085-1095. DOI： 10.19969/j.fxcsxb.23032501.

摘要

为有效解决霜膏类化妆品中风险物质“检不全，检不快”的问题，建立了化妆品中297种风险物质的QuEChERS结合高效液相色谱-四极杆-飞行时间质谱（HPLC-Q-TOF MS）的快速筛查方法。样品经饱和氯化钠分散，无水乙醇提取，C,18,分散固相萃取，采用HPLC-Q-TOF MS测定。基于超高效液相色谱-三重四极杆串联质谱（UPLC-MS/MS），选择45种风险物质作为质控化合物对QuEChERS方法进行优化，方法检出限（LOD）为0.01~0.20 mg/kg，定量下限（LOQ）为0.04~0.40 mg/kg，3个加标水平（低、中、高）的平均回收率为81.5%~117%，相对标准偏差（RSD，,n,=6）为2.0%~14%。将QuEChERS方法扩展应用至297种风险物质的HPLC-Q-TOF MS靶向筛查，收集化合物的一级和二级质谱信息，建立高分辨率质谱筛查表，通过比对HPLC-Q-TOF MS采集的信息与筛查表锁定“可疑目标物”，进一步利用UPLC-MS/MS定量确证。应用此法对29个霜膏类样品进行靶向筛查，检出甲芬那酸、盐酸赛庚啶、克林霉素、林可霉素，含量为0.042~3 180 mg/kg。该方法的建立可为化妆品中风险物质的快速筛查提供技术依据。

Abstract

In order to effectively solve the problem of“incomplete and slow detection”of risk substances in cream cosmetics，a rapid screening method for 297 risk substances in cosmetics using QuEChERS combined with high-performance liquid chromatography quadrupole time of flight mass spectrometry（HPLC-Q-TOF MS） was established. The sample was dispersed with saturated sodium chloride，extracted with anhydrous ethanol，extracted with C,18 ,dispersion solid phase extraction，and determined by HPLC-Q-TOF MS. The optimization of QuEChERS method is based on ultra high performance liquid chromatography triple quadrupole tandem mass spectrometry（UPLC-MS/MS） technology. 45 risk substances were selected as quality control compounds，with limits of detection（LODs） of 0.01 mg/kg to 0.20 mg/kg，and limits of quantitation（LOQs） of 0.04 mg/kg to 0.40 mg/kg. Average recoveries for the three spiked levels（low，medium and high） were in range of 81.5%-117%，with relative standard deviations（RSDs，,n=,6） of 2.0% to 14%. The QuEChERS method was extended to the HPLC-Q-TOF MS targeted screening of 297 risk substances，namely，collecting the primary and secondary mass spectrometry informations of compounds，establishing a high-resolution mass spectrometry screening table，and comparing the informations collected by HPLC-Q-TOF MS with the screening table to identify“suspicious targets”，further using UPLC-MS/MS for quantitative confirmation. 29 cream samples were targeted and screened with this method，and mefenamic acid，cyproheptadine hydrochloride，clindamycin and lincomycin were screened，with the detection amount of 0.042-3 180 mg/kg. The method provides a technical basis for rapid screening of risk substances in cosmetics.

关键词

化妆品QuEChERSHPLC-Q-TOF MSUPLC-MS/MS风险物质

Keywords

cosmeticsQuEChERSHPLC-Q-TOF MSUPLC-MS/MSrisk substances

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