固相萃取净化-超高效液相色谱-三重四极杆/线性离子阱串联质谱法测定化妆品中16个卡因类组分  

Determination of 16 caine-type ingredients in cosmetics by UPLC-QQQ/LIT tandem mass spectrometry coupled with solid phase extraction

作　　者：芦丽 方方 冯有龙 曹玲 LU Li;FANG Fang;FENG You-long;CAO Ling(Jiangsu Institute for Food and Drug Control,Nanjing 210008,China)

机构地区：[1]江苏省食品药品监督检验研究院,南京210008

出　　处：《药物分析杂志》2021年第12期2178-2190,共13页Chinese Journal of Pharmaceutical Analysis

基　　金：江苏省市场监督管理局科技计划项目(KJ207560)。

摘　　要：目的:建立了固相萃取柱净化,超高效液相色谱-三重四极杆/线性离子阱串联质谱联用(UPLC-MS/MS)测定化妆品中添加的16个卡因类组分的方法。方法:不同基质样品用溶剂提取后,经Oasis MCX固相萃取柱净化,采用ACE Excel 3 C_(18)(150 mm×2.1 mm,3.0μm)分离16个卡因类组分,以甲醇-0.1%甲酸溶液为流动相进行梯度洗脱。在电喷雾离子源(ESI)正离子模式下电离,多反应监测(MRM)模式下定量和线性离子阱增强子离子扫描(EPI)模式下定性。结果:16个卡因类组分在相应的测定范围内线性关系良好,相关系数(r)在0.9995~1.000,在2个加标水平下,加标回收率范围为86.0%~113.2%,RSD(n=3)为0.9%~10.8%,各化学成分的检测下限在2~5μg·kg^(-1)。收集的59批次化妆品中15批次检出丙胺卡因、利多卡因、丁卡因,含量在16.4~150.2 mg·g^(-1)。结论:该方法简便,选择性好,灵敏度高,可用于化妆品中卡因类化学成分的定量测定和定性筛查。Objective:To develop a method based on SPE-UPLC-MS/MS[solid phase extraction-ultraper-formance liquid chromatography(UPLC)-triple quadrupole mass spectrometry(QQQ)/linear accelerated ion trap(LIT)tandem mass spectrometry mass spectrometry]for determination of 16 caine-type ingredients in cosmetics.Methods:Samples were extracted with solvent and then purified with an Oasis MCX column.16 compounds were separated on an ACE Excel 3 C_(18)(150 mm×2.1 mm,3.0μm)column with 0.1%formic acid solution-methanol as mobile phases by gradient elution.Detection was carried out by positive electrospray ionization(ESI^(+))mass spectrometer in multiple reaction monitor(MRM)mode for quantification and enhanced product ion(EPI)scan for qualification.Results:All the 16 caine-type ingredients showed good linearity in their reasonableranges(r=0.9995-1.000).The average recoveries of all compounds at two spiked levels were in the range of 86.0%-113.2%with RSDs(n=3)within 0.9%-10.8%.The LODs were all in the range of 2-5μg·kg^(-1).Lidocaine,prilocaine and tracaine were found in 15 batches of the 59 tested samples.The contents were in range of 16.4-150.2 mg·g^(-1).Conclusion:With the advantages of rapidness,simplicity,good selectivity and high sensitivity,the method can be used for determination of caine-type ingredients in cosmetics.

关 键 词：固相萃取 超高效液相相色谱-质谱联用法 线性离子阱 增强子离子扫描 卡因类局麻药物 化妆品 

分 类 号：R917[医药卫生—药物分析学]