摘要
目的建立12种准用染发剂的高效液相色谱测定方法及液相色谱-串联质谱确证分析方法。方法样品经2 g/L亚硫酸氢钠水溶液和无水乙醇(1+1,体积比)的混合溶液超声提取,采用菲罗门Titank C_(18)(4.6 mm×250 mm,5μm)分离,以10 mmol/L磷酸氢二钾液(磷酸调pH值为7.5)-甲醇-乙腈为流动相梯度洗脱,二级阵列管检测器(DAD)在280 nm测定,外标法定量,采用液相色谱-串联质谱法进行确证。结果12种染发剂在1μg/ml~200μg/ml线性良好,相关系数均>0.999,方法检出浓度(LOD)为5μg/g~50μg/g,方法定量浓度(LOQ)为17μg/g~167μg/g,3个水平加标回收率为90.1%~104.5%,相对标准偏差(RSD)为0.4%~4.2%。结论本研究建立的方法准确、快速、简便,对疑似阳性样品可进一步采用质谱确证,有效避免假阳性结果,适用于化妆品中12种染发剂的准确测定。
Objective To establish a method for the determination of 12 hair dyes by high performance liquid chromatography(HPLC)and liquid chromatography-tandem mass spectrometry(LC-MS/MS).Methods The samples were extracted by ultrasonic with a mixed solution of 2 g/L sodium bisulfite aqueous solution and anhydrous ethanol(1+1),and separated on a Phenomenex Titan Ccolumn(4.6 mm×250 mm,5μm),gradient evolution with 10 mmol/L dipotassium hydrogen phosphate solution(adjusted pH 7.5 by phosphoric acid)-methanol-acetonitrile as mobile phase.The detection wavelength was 280 nm,and the samples were quantified by external standard method.The suspected samples were further verified by liquid chromatography-tandem mass spectrometry(LC-MS/MS).Results Twelve hair dyes had a good linearity in the range of 1μg/ml-200μg/ml with correlation coefficients(r)larger than 0.999.The limits of detection(LODs)were between 5μg/g and 50μg/g and the limits of quantitation(LOQs)were between 17μg/g and 167μg/g.The spiked recoveries were within 90.1%-104.5%,with the relative standard deviation(RSD)of 0.4%-4.2%.Conclusion The method is accurate,rapid and simple.The suspected positive samples can be further confirmed by mass spectrometry,which can effectively avoid false positive results.It is suitable for the determination of 12 hair dyes in cosmetics.
作者
吴思霖
彭兴盛
郑荣
WU Si-lin;PENG Xing-sheng;ZHENG Rong(Shanghai Institute for Food and Drug Control,National Medical Products Administration Key Laboratory for Monitoring and Evaluation of Cosmetics,Shanghai 201203,China)
出处
《中国卫生检验杂志》
CAS
2022年第14期1665-1670,共6页
Chinese Journal of Health Laboratory Technology
基金
上海市科学技术委员会科技计划项目(21142202700)。
关键词
染发剂
化妆品
高效液相色谱法
液相色谱-串联质谱法
Dyes
Cosmetics
High performance liquid chromatography
Liquid chromatography-tandem mass spectrometry
