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.
作者
陈静
毛北萍
郑荣
王柯
CHEN Jing;MAO Bei-ping;ZHENG Rong;WANG Ke(Shanghai Institute of Food and Drug Control,Shanghai 201203,China)
出处
《日用化学工业》
CAS
CSCD
北大核心
2018年第12期717-724,共8页
China Surfactant Detergent & Cosmetics
