Determination of Fifteen N-nitrosamine Compounds in Cosmetics by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

WANG Yi; LIANG Wen-yao; HE Guo-shan; CHEN Zhang-hao; ZHOU Zhi-ming; WU Qian; XI Shao-feng; TAN Jian-hua

doi:10.19969/j.fxcsxb.23051602

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Determination of Fifteen N-nitrosamine Compounds in Cosmetics by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

Scientific Papers | 更新时间：2023-11-10

- Determination of Fifteen N-nitrosamine Compounds in Cosmetics by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
- Journal of Instrumental Analysis Vol. 42, Issue 11, Pages: 1469-1478(2023)
- 作者机构：
  
  1.广州质量监督检测研究院，国家化妆品质量检验检测中心（广州），广东广州 511447
  2.广东省药品检验所，广东广州 510663
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.23051602
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汪毅,梁文耀,何国山等.超高效液相色谱-串联质谱法测定化妆品中15种N-亚硝胺化合物[J].分析测试学报,2023,42(11):1469-1478.

WANG Yi,LIANG Wen-yao,HE Guo-shan,et al.Determination of Fifteen N-nitrosamine Compounds in Cosmetics by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(11):1469-1478.
汪毅,梁文耀,何国山等.超高效液相色谱-串联质谱法测定化妆品中15种N-亚硝胺化合物[J].分析测试学报,2023,42(11):1469-1478. DOI： 10.19969/j.fxcsxb.23051602.

WANG Yi,LIANG Wen-yao,HE Guo-shan,et al.Determination of Fifteen N-nitrosamine Compounds in Cosmetics by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(11):1469-1478. DOI： 10.19969/j.fxcsxb.23051602.

摘要

采用超高效液相色谱-串联质谱（UPLC-MS/MS）建立了化妆品中15种痕量N-亚硝胺化合物的分析方法。水剂样品以水或乙腈分组超声提取，膏霜乳液样品采用亚铁氰化钾-乙酸锌溶液沉淀大分子或者饱和氯化钠-乙腈盐析分组处理后，以Agilent Poroshell 120 SB-Aq（100 mm×3.0 mm，2.7 μm）色谱柱分离，经大气压化学电离源（APCI）电离，多反应监测模式检测，以同位素内标法定量。结果表明，15种N-亚硝胺化合物在相应质量浓度范围内线性关系良好（,r,2,＞0.995），检出限和定量下限分别为5~15 ng/g和15~45 ng/g。水、乳、膏霜3种化妆品基质在25、50、100 ng/g加标水平下的平均回收率为88.0%~111%，相对标准偏差（RSD，,n,=6）为1.4%~9.8%。该方法用于市售化妆品检测，发现13批次样品检出N-亚硝基二乙醇胺（NDELA），其中1批次超限量值。方法的专属性强，灵敏度高，精密度好，解决了N-亚硝胺化合物稳定性差、易被干扰等问题，适用于化妆品中15种N-亚硝胺化合物的痕量测定。

Abstract

An ultra performance liquid chromatography-tandem mass spectrometric（UPLC-MS/MS） method was established for detecting 15 trace N-nitrosamine compounds in cosmetics. The final established method involved ultrasonic extraction of cosmetics using water or acetonitrile for different compounds. The samples were treated with potassium ferrocyanide-zinc acetate solution for precipitating macromolecules or saturated sodium chloride-acetonitrile for salting out. An Agilent Poroshell 120 SB-Aq（100 mm × 3.0 mm，2.7 μm） chromatography column was used for separation，followed by atmospheric pressure chemical ionization（APCI） source and multiple reaction monitoring mode detection in the isotope internal standard method for quantification. The result showed good linearity（,r,2,>,0.995） for the 15 N-nitrosamine compounds in their respective concentration ranges，with detection and quantitation limits of 5-15 ng/g and 15-45 ng/g，respectively. The average recoveries for the three cosmetic matrices（aqueous，emulsion，cream） at spiked levels of 25，50，100 ng/g were between 88.0% and 111%，with relative standard deviations（RSD，,n,=6） of 1.4%-9.8%. The method was applied to the detection of commercial cosmetics and N-nitrosodiethanolamine（NDELA） was detected in 13 batches，with one batch exceeding the limit. The strong specificity，high sensitivity，and good precision made the method could solve the problems of poor stability and easy interference of N-nitrosamine compounds，and was suitable for the trace determination of 15 N-nitrosamine compounds in cosmetics.

关键词

N-亚硝胺化合物化妆品超高效液相色谱-串联质谱法（UPLC-MS/MS）大气压化学电离源

Keywords

N-nitrosamine compoundscosmeticsultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）atmospheric pressure chemical ionization（APCI） source

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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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