高级检索

    高效液相色谱法测定氧化型染发产品中2-氨基-4-羟乙氨基茴香醚及其硫酸盐的含量

    Determination of 2-Amino-4-Hydroxyethylaminoanisole and Its Sulfate in Oxidative Hair Dye Products by High Performance Liquid Chromatography

    • 摘要: 建立了高效液相色谱法(HPLC)测定氧化型染发产品中2-氨基-4-羟乙氨基茴香醚及其硫酸盐含量的方法,并采用高效液相色谱-串联质谱法(HPLC-MS/MS)对目标物进行定性确证。称取染发膏0.5 g于比色管中,用体积比为3:7的2.5 g·L-1 L-半胱氨酸溶液(抗氧化剂)-乙醇的混合液提取并定容至10 mL。以Waters Atlantis® T3 MV Kit色谱柱为固定相,以含10%(体积分数)乙腈的磷酸盐缓冲溶液-乙腈的混合液为流动相进行梯度洗脱,利用二极管阵列检测器,于304 nm对样品溶液进行测定。HPLC-MS/MS确证分析中采用电喷雾正离子源(ESI+)和多反应监测(MRM)模式,当供试品中出现质荷比(m/z)183.0>138.0和m/z 183.0>95.2两个离子对,且离子对间的相对丰度比在允许偏差±20%以内时,可确认供试品中含有2-氨基-4-羟乙氨基茴香醚(硫酸盐)。结果显示:2-氨基-4-羟乙氨基茴香醚的质量浓度在1.984~496.1 mg·L-1内与其对应的峰面积呈线性关系,检出限(3S/N)为8 μg·g-1,以2-氨基-4-羟乙氨基茴香醚硫酸盐计,检出限(3S/N)为12 μg·g-1;不同质量浓度的2-氨基-4-羟乙氨基茴香醚基质匹配标准溶液在24 h内的峰面积的相对标准偏差(RSD,n=7)均小于1.0%;对空白基质样品和染发膏样品进行加标回收试验,回收率为95.5%~101%,测定值的RSD (n=6)为1.9%~2.4%。方法用于7个染发产品分析,其中5个样品中检出2-氨基-4-羟乙氨基茴香醚硫酸盐,检出量为0.053 6%~0.369 0%,与HPLC-MS/MS的确证结果一致;其余2个样品中未检出,与标示内容不相符。

       

      Abstract: A method for determination of 2-amino-4-hydroxyethylaminoanisole and its sulfate in oxidative hair dye products by high performance liquid chromatography (HPLC) was established, and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was used for qualitative verification. 0.5 g of hair dye cream was put into a colorimetric tube and extracted with a mixture of 2.5 g·L-1 L-cysteine solution (used as the antioxidant) and ethanol at volume ratio of 3:7, and the volume was fixed to 10 mL with the above mixture. Waters Atlantis® T3 MV Kit chromatographic column was used as stationary phase, and a mixture of the phosphate buffer solution containing 10% acetonitrile and acetonitrile was used as mobile phase for gradient elution. The sample solution was determined at 304 nm by diode array detector. ESI+ and MRM mode were used for HPLC-MS/MS analysis verification. When ion pairs of m/z 183.0>138.0 and m/z 183.0>95.2 were appeared in tested sample, and the deviation of the relative abundance ratio of ion pairs was within ±20%, 2-amino-4-hydroxyethylaminoanisole (sulfate) was confirmed in the tested sample. As shown by the results, linear relationship between mass concentration of 2-amino-4-hydroxyethylaminoanisole and its peak area was kept in the range of 1.984-496.1 mg·L-1, with detection limits of 8 μg·g-1 for 2-amino-4-hydroxyethylaminoanisole and 12 μg·g-1 for 2-amino-4-hydroxyethylaminoanisole sulfate. RSDs (n=7) of peak areas of 2-amino-4-hydroxyethylaminoanisole matrix matching standard solutions with different mass concentrations in 24 h were less than 1.0%. Recovery test was made on blank matrix sample and hair dye sample by standard addition method, giving results in the range of 95.5%-101%, and RSDs (n=6) of the determined values were ranged from 1.9% to 2.4%. This method has been applied for analysis of 7 hair dye products. 2-Amino-4-hydroxyethylaminoanisoleand sulfate was detected in 5 samples, with the detection amounts in the range of 0.053 6%-0.369 0%, which was consistent with HPLC-MS/MS verification results, while it was not detected in the other 2 samples, which was inconsistent with the labeling content.

       

    /

    返回文章
    返回