高效液相色谱-质谱联用法同时测定8种不同基质类型化妆品中的23种防腐剂  

Simultaneous determination of 23 preservatives in 8 different matrixes of cosmetics by HPLC-MS/MS

作　　者：陈静[1] 毛北萍[1] 郑荣[1] 王柯[1] CHEN Jing;MAO Bei-ping;ZHENG Rong;WANG Ke(Shanghai Institute of Food and Drug Control,Shanghai 201203,China)

机构地区：[1]上海市食品药品检验所,上海201203

出　　处：《日用化学工业》2018年第12期717-724,共8页China Surfactant Detergent & Cosmetics

摘　　要：建立了同时测定8种不同基质类型的化妆品中23种防腐剂的高效液相色谱-质谱联用法(HPLC-MS/MS)。样品经溶剂超声提取,以10 000 r/min离心5 min,经0. 22μm微孔滤膜过滤后取续滤液测定。采用Agilent Poroshell 120EC-C_(18)柱(100 mm×4. 6 mm,2. 7μm),以5 mmol/L乙酸铵水溶液-5 mmol/L乙酸铵甲醇溶液梯度洗脱,流速0. 45 m L/min,柱温30℃,进样量2μL,采用三重四级杆质谱测定。结果表明,方法的相对标准偏差为0. 6%～8. 4%;回收率为76. 3%～107. 1%;各种防腐剂的线性范围不同,分别在1～100,10～1 000和100～10 000μg/L的质量浓度范围内呈良好线性关系,相关系数均大于0. 996; 23种防腐剂的方法检出限为0. 04～4μg/g。该方法具有分离效率高、分析时间短、分析成分多等特点,适用于实际样品的测定。A high liquid chromatography tandem mass spectrometric(HPLC-MS/MS)method has been developed for the simultaneous determination of 23 preservatives in 8 different matrixes of cosmetics.Samples were ultrasonically extracted by solvent,centrifuged at 10 000 r/min for 5 min,filtered through a 0.22μm microporous membrane,and the continued filtrate was taken for analysis.The separation was carried out by an Agilent Poroshell 120 EC-C 18 column(100 mm×4.6 mm,2.7μm)with a gradient elution of 5 mmol/L ammonium acetate in water and 5 mmol/L ammonium acetate in methanol.The flow rate was 0.45 mL/min,the column temperature was 30℃,and the injection volume was 2μL.A triple quadrupole tandem mass spectrometric method was used as the determination method.The results show that the relative standard deviations(RSD)are 0.6%-8.4%,the recoveries are 76.3%-107.1%,the linear range of various preservatives is different ranging from 1-100,10-1 000 and 100-10 000μg/L.The linear mass concentration has a good linear relationship,and the correlation coefficient is greater than 0.996.The detection limits of 23 preservatives are 0.04-4μg/g.This method has the advantages of high separation efficiency,short analysis time and many analytical components,and is suitable for analyzing the preservatives in cosmetics products.

关 键 词：化妆品 高效液相色谱-质谱联用法 防腐剂 

分 类 号：TQ658[化学工程—精细化工]