液相色谱串联质谱法同时测定6类不同剂型化妆品中10种防腐剂  

Simultaneous determination of 10 preservatives in 6 different dosage forms of cosmetics by HPLC-MS/MS

作　　者：符策奕[1] 梁颖[1] 许文佳[1] 陈朝曼[1] 

机构地区：[1]海南省药品检验所,海口570216

出　　处：《药物分析杂志》2016年第8期1456-1464,共9页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立液相色谱串联质谱同时测定6类不同剂型化妆品中10种防腐剂的定性、定量方法。方法:半固体或固体样品经有机溶剂超声提取,HLB固相萃取柱分离,有机滤膜过滤,再通过Phenomenex Kinetex C18色谱柱(100 mm×2.1 mm,2.6μm)分离,柱温为35℃,流速为0.3 m L·min^(-1),流动相:甲醇(A)-水(B),梯度洗脱(0~13 min,35%A→65%A;13~14 min,65%A→88%A;14~20 min,88%A;20~21 min,88%A→35%A;21~30 min,35%A)。采用电喷雾离子源及多反应监测模式(MRM)对目标化合物进行测定。液体样品则无需采用HLB固相萃取柱分离,其余步骤与半固体和固体样品一致。结果:甲基异噻唑啉酮、甲基氯异噻唑啉酮、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、对羟基苯甲酸异丙酯、对羟基苯甲酸丁酯、对羟基苯甲酸异丁酯、三氯生、三氯卡班的方法检出限分别为0.79、0.73、0.65、0.42、0.41、1.0、0.42、0.40、2.0、2.0 mg·kg^(-1);10种防腐剂在一定的浓度范围内线性关系良好(r>0.999 0),在6类不同剂型的化妆品中回收率在90%~108%范围内。18批不同类型的化妆品样品中共有2批异噻唑啉酮类添加量超过《化妆品卫生规范》(2007版)规定。结论:该方法经方法学验证,适用于化妆品中10种防腐剂的同时测定。Objective： To develop an HPLC-MS/MS method for simultaneous determination of 10 preservatives in 6 different dosage forms of cosmetics. Methods： The semisolid or solid cosmetic sample was extracted with organic solvents under uhrasonication, separated by HLB solid phase extraction, and then filtered by organic filter membrane. The analytes were separated on a Phenomenex Kinetex ClS column （ 100 mm× 2. 1 mm, 2. 6 μm ）with gradient elution at a flow rate of 0. 3 mL.min^-1. The mobile phase consisted of methanol （ A ） and water （ B ） with gradient elution（0-13 min, 35%A→ 65%A; 13-14 min, 65%A → 88%A; 14-20 min, 88%A; 20-21 min, 88%A → 35%A; 21-30 min, 35%A ）. The column temperature was 35 ℃. The compounds were identified under electrospray ionization and multiple reactions monitoring （ MRM ） mode. The liquid cosmetics do not need to be separated by HLB solid phase extraction, and the other steps are consistent with the semisolid and solid cosmetics. Results ： The LODs of methylisothiazolinone, methylchloroisothiazolinone, methylparaben, ethylparaben, propylparaben, isopropyl paraben, butyl paraben, isobutyl paraben, triclosan and triclocarban were 0. 79, 0.73,0.65, O. 42, 0.41,1.0,0.42,0.40, 2.0 and 2. 0 mg. kg-1, respectively. In a certain range, the calibration curves for 10 preservatives were liner and the correlation coefficients were above 0. 999 0. The recoveries of 10 preservatives in 6 different dosage forms of cosmetics ranged from 90% to 108%. 2 batches of isothiazolinone adding amount exceeds the regulations of Hygienic Standard for Cosmetic （ 2007 edition ）among the 18 batches of different types of cosmetic samples. Conclusion： The method has validated by methodology and it is suitable for the simultaneous determination of 10 preservatives in cosmetics.

关 键 词：防腐剂 化妆品 甲基异噻唑啉酮 甲基氯异噻唑啉酮 对羟基苯甲酸甲酯 对羟基苯甲酸乙酯 对羟基苯甲酸丙酯 对羟基苯甲酸异丙酯 对羟基苯甲酸丁酯 对羟基苯甲酸异丁酯 三氯生 三氯卡班 液相色谱串联质谱 

分 类 号：R917[医药卫生—药物分析学]