摘要
氧化型染发产品中的多种染发剂具有不同程度的致敏性及其他毒性,建立快速、准确检测多种染发剂的方法,为该类产品监管提供有效的技术手段,十分必要。该研究建立了氧化型染发类产品中40种染发剂的高效液相色谱测定方法。染发产品经含70%乙醇的亚硫酸氢钠水溶液涡旋、超声提取,并经亚硫酸氢钠水溶液稀释后,以0.02 mol/L乙酸铵水溶液(含4%乙腈)和乙腈为流动相,采用Waters AtlantisT3 MV Kit色谱柱(250 mm×4.6 mm,5μm)分离,配合柱温变化进行梯度洗脱,二极管阵列检测器检测,检测波长为235 nm和280 nm,外标法定量。结果表明,40种染发剂在各自范围内线性关系良好,相关系数均大于0.999;40种染发剂的检出限为5~168μg/g,定量限为16~504μg/g;各染发剂在3个添加水平下的平均回收率为81.4%~109.6%,RSD均小于5%;各染发剂标准溶液在24 h内稳定性良好,RSD为0.2%~2.2%。与现行标准检验方法相比,该方法较大程度地增加了单一液相色谱条件下可测定的染发剂,特别是准用染发剂种类(36种),提高了检测效率,并可保证检测结果的灵敏度与准确性,适用于氧化型染发产品中多种染发剂的检测分析。
Oxidative hair dye products have always been one of the key concerns in cosmetic supervision.The various aromatic amine and phenol dyes used in such products have different degrees of sensitization and toxicities.Therefore,it is necessary to establish a rapid and accurate method for the determination of various dyes.A high performance liquid chromatography(HPLC)method was developed for the determination of 40 dyes in oxidative hair dye products,and the method was optimized in terms of mobile phase type,column temperature,detection wavelength,and extraction solvent concentration.The sample pretreatment method was as follows:weighed 0.5 g sample accurately,added to 10 mL of sodium bisulfite solution containing 70%ethanol,extracted by ultrasonication for 15 min,added to 25 mL of the sodium bisulfite solution.Chromatographic separation was carried out on a Waters AtlantisT3 MV Kit column(250 mm×4.6 mm,5μm)by gradient elution.To protect the column,the sample solution was filtered using a syringe filter with a 0.45-μm membrane before injection.The mobile phase was 0.02 mol/L ammonium acetate aqueous solution(containing 4%acetonitrile)and acetonitrile.The column temperature was varied between 30℃and 35℃during the separation.The dyes were detected using a photodiode array detector.The detection wavelength of 31 dyes was 235 nm,and that of the other nine dyes was 280 nm.The external standard method was used for quantitative analysis.The results showed that the 40 dyes could be separated well.All the dyes had good linearities in their own concentration ranges,with correlation coefficients(r)exceeding 0.999.The limits of detection(LODs)of the 40 dyes ranged from 5 to 168μg/g,and the limits of quantification(LOQs)ranged from 16 to 504μg/g.The average spiked recoveries at three levels(2.5,5.0,and 10 mg/g)of the 40 dyes ranged from 81.4%to 109.6%,with relative standard deviations(RSDs)less than 5%.The stability of each dye in the standard solutions was good within 24 h,with RSDs ranging from 0.2%to 2.2%.To demonstr
作者
左雪
邸铮
杜勇
杨玲
张蓉
邬国庆
ZUO Xue;DI Zheng;DU Yong;YANG Ling;ZHANG Rong;WU Guoqing(Beijing Institute for Drug Control, Beijing 102206, China)
出处
《色谱》
CAS
CSCD
北大核心
2021年第11期1222-1229,共8页
Chinese Journal of Chromatography
关键词
高效液相色谱
染发剂
氧化型染发产品
high performance liquid chromatography(HPLC)
dyes
oxidative hair dye products
