高效液相色谱法与液质联用仪法同时测定15批次化妆品中5种限用防腐剂的比较研究  

A Comparative Study of Simultaneous Determination of Five Impermissible Preservatives in 15 Batches of Cosmetics by HPLC and HPLC-MS Methods

作　　者：漆爱明 毛丽秋[2] 肖树雄[1] 余燕[1] QI Ai-ming;MAO Li-qiu;XIAO Shu-xiong;YU Yan(Guangdong Institue for Drug Control,Guangzhou 510300,China;College of Chemistry and Chemical Engineering,Hunan Normal University,Changsha 410081,China)

机构地区：[1]广东省药品检验所,中国广州510300 [2]湖南师范大学化学化工学院,中国长沙410081

出　　处：《湖南师范大学自然科学学报》2020年第1期56-62,共7页Journal of Natural Science of Hunan Normal University

基　　金：广东省科技计划资助项目(2016A040403076)

摘　　要：应用高效液相色谱法和液相色谱质谱联用仪法分别建立了对2种基质类型化妆品中限用防腐剂氯己定、苄氯酚、氯二甲酚、o-苯基苯酚和p-氯-m-甲酚的测定方法。样品经溶剂超声提取,以8000 r/min离心15 min,经0.45μm(液相色谱)/0.22μm(液质联用仪)微孔滤膜过滤后取续滤液测定。两种分析方法分别采用不同的色谱柱、不同的洗脱溶剂和不同的洗脱程序进行测定。结果表明高效液相色谱法和液相色谱质谱联用仪测定氯己定等5种限用防腐剂在不同线性范围内线性关系分别良好,线性相关系数均大于0.990。方法精密度的相对标准偏差分别为0.4%~1.1%和1.0%~2.8%;回收率分别为103.7%~119.8%和71.2%~117.2%;5种防腐剂的方法检出限分别为2.10~4.70μg/g和1.05~2.45μg/g。实验数据表明液质联用仪法更适合于化妆品中5种限用防腐剂的定性测定,液相色谱法适用于样品的定量测定。A high performance liquid chromatography(HPLC) method combined with a High Performance Liquid Chromatography-tandem Mass Spectrometry(HPLC-MS) method has been developed in this work for the simultaneous determination of five impermissible substances, chlorhexidine, 2-benzyl-4-chlorophenol, 4-chloro-3,5-dimethyphenol, 2-phenylphenol, and 4-chloro-3-methylphenol, in 2 different matrixes of cosmetics. Samples were ultrasonically extracted by solvent, centrifuged at 8 000 r/min for 15 min, and then filtered through a 0.45 microporous membrane(HPLC-MS with 0.22 μm microporous membrane). Our results show that mass concentrations obtained from HPLC and HPLC-MS methods possess strong linear relationship with the correlation coefficient better than 0.990, but their linearity range of five preservatives is different. The relative standard deviations(RSD) of the two methods is 0.4%~1.1% and 1.0%~2.8%, respectively. Their recoveries are 103.7%~119.8% and 71.2%~117.2%, and detection limits 2.10~4.70 μg/g and 1.05~2.45 μg/g, respectively. This work demonstrates that HPLC-MS is suitable for the qualitative analysis but HPLC is suitable for the quantitative analysis of the preservatives in cosmetics products.

关 键 词：化妆品 限用防腐剂 高效液相色谱(HPLC) 液相色谱质谱联用仪(HPLC-MS) 

分 类 号：O657.72[理学—分析化学] TS255.53[理学—化学]