摘要
目的建立同时测定化妆品中苄索氯铵、十六烷基二甲基苄基氯化铵、十四烷基二甲基苄基氯化铵、十二烷基二甲基苄基氯化铵、脱氢乙酸、甲基氯异噻唑啉酮、甲基异噻唑啉酮、山梨酸、三氯卡班、4-羟基苯甲酸丙酯、4-羟基苯甲酸异丙酯、4-羟基苯甲酸丁酯、4-羟基苯甲酸异丁酯、4-羟基苯甲酸乙酯、4-羟基苯甲酸甲酯及苯甲酸16种防腐剂的高效液相色谱-串联质谱检测方法。方法样品经甲醇溶液超声提取后,采用高效液相色谱-串联质谱进行测定。采用Agilent Zorbax SB-C18色谱柱(2.1 mm×100 mm,1.8μm),流动相A为5 mmol/L乙酸铵的水溶液,流动相B为含5 mmol/L乙酸铵的甲醇,梯度洗脱;流速为0.3 ml/min;进样量为2μl;柱温为30℃。结果 16种防腐剂线性范围为1 ng/ml^100 ng/ml(r>0.995),检出限<0.001%,平均回收率为75.3%~105.6%,RSD为0.4%~5.8%。结论该方法快速简便,适用于化妆品中4-羟基苯甲酸酯类等16种防腐剂的快速筛查。
Objective To develop a liquid chromatography tandem mass spectrometry（ LC-MS / MS） method for the simultaneous determination of benzethonium chloride,benzylhexadecyl dimethylammonium chloride,tetradecyl dimethyl benzyl ammonium chloride,dodecyl dimethyl benzyl ammonium chloride,dehydroacetic acid,methylisothiazolinone（ MIT）,methylchloroisothiazolinone（ CMIT）,sorbic acid,triclocarban,methyl 4-hydroxybenzoate,ethyl 4-hydroxybenzoate,propyl p-hydroxybenzoate,isopropyl 4-hydroxybenzoate,butyl paraben,isopropyl 4-hydroxybenzoate,benzoic acid in cosmetics. Methods The samples were ultrasonically pretreated with methanol and detected by LC-MS / MS. The separation was carried out on an Agilent Zorbax SB-C18column（ 2. 1 mm × 100 mm,1. 8 μm） in a gradient elution mode,with 5 mmol / L ammonium acetate aqueous solution as mobile phase A and 5 mmol / L ammonium acetate methanol solution as mobile phase B. The flow rate was0. 3 ml / min; the injection volume was 2 μl and the column temperature was 30 ℃. Results Good linearity was obtained when the concentrations of preservatives were within 1 ng / ml-100 ng / ml（ r 〉 0. 995）,with the average recoveries of 75. 3%-105. 6%,the limits of detection 〈 0. 001% and relative standard deviation（ RSD） within 0. 4%-5. 8%. Conclusion The method is simple,rapid and accurate. It was suitable for the rapid screening of 16 kinds of preservatives in cosmetics,such as4-hydroxy benzoic acid ester.
出处
《中国卫生检验杂志》
CAS
2016年第19期2758-2761,共4页
Chinese Journal of Health Laboratory Technology
关键词
防腐剂
化妆品
液相色谱-串联质谱法
Preservative
Cosmetics
Liquid chromatography tandem mass spectrometry
