UPLC-MS/MS法测定化妆品中5种美白剂  

Determination of 5 whitening agents in cosmetics using UPLC-MS/MS

作　　者：王昌钊 李子豪 王一欣 杨玥 Changzhao Wang;Zihao Li;Yixin Wang;Yue Yang(Xi’an Customs Technology Center,Xi’an,Shaanxi 710068,China;Shaanxi Institute for Food and Drug Control,Xi’an,Shaanxi 710065,China;CCIC Shaanxi Co.,Ltd.,Xi’an,Shaanxi 710068,China)

机构地区：[1]西安海关技术中心,陕西西安710068 [2]陕西省食品药品检验研究院,陕西西安710065 [3]中国检验认证集团陕西有限公司,陕西西安710068

出　　处：《日用化学工业（中英文）》2024年第7期873-878,共6页China Surfactant Detergent & Cosmetics

基　　金：陕西省重点研发计划项目资助(2022GY-321)。

摘　　要：建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)测定化妆品中5种美白剂的方法。样品采用甲醇-水(70∶30)溶液作为提取溶剂,超声提取30 min,采用ZORBAX RR StableBond Aq(Agilent)色谱柱进行液相分离,梯度洗脱,采用电喷雾离子源负离子模式扫描和多反应监测模式采集。结果表明,在最优条件下,5种美白成分实现有效分离,以水乳、霜膏、粉饼化妆品为基质的标准工作曲线均在1.0~200.0 ng/mL范围内线性良好,相关系数R^(2)≥0.996,方法检出限为0.01~0.1 mg/kg,定量限为0.03~0.3 mg/kg。3种不同基质的化妆品样品在1倍、2倍、10倍定量限浓度加标的平均回收率为82.6%~104.8%,相对标准偏差为2.1%~8.6%(n=6)。该方法操作简便,准确性良好,适用于不同基质化妆品中脱氧熊果苷、α-熊果苷、β-熊果苷、对苯二酚和熊果酸5种美白剂的测定。A method was established for quantitative determination of five whitening agents in cosmetics using ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The samples were extracted with methanol-water solution(70∶30),ultrasonic extraction for 30 minutes and then separated by Agilent column(ZORBAX RR StableBond Aq)followed by gradient elution.An electrospray ionization(ESI)source in negative ion mode was utilized for multiple reaction monitoring(MRM)scanning.The results show that under optimal conditions no obvious matrix effect exists in 3 different cosmetic matrices.Among the three cosmetics with different types of matrices,good linearity is obtained for five whitening agents in the range of 1.0-200.0 ng/mL,and the correlation coefficients(R^(2))are more than 0.996.The limit of detection(LOD)and limit of quantitation(LOQ)are 0.01-0.1 mg/kg and 0.03-0.3 mg/kg,respectively.Spike recovery is performed on three cosmetics at three different spike levels(1,2,and 10 times of the LOQ),and the average recovery range is 82.6%-104.8%with a relative standard deviation of 2.1%-8.6%(n=6).This method is easy to implement,efficient and accurate.It is suitable for quantitative analysis of five whitening agents,including deoxyarbutin,α-arbutin,β-arbutin,hydroquinone,and ursolic acid in common cosmetics,providing technical support for the regulation and risk monitoring of the cosmetics industry.

关 键 词：超高效液相色谱-四极杆串联质谱法 美白剂 化妆品 

分 类 号：TQ658[化学工程—精细化工]