高效液相色谱法同时测定氧化型染发产品中33种染发剂

建立了高效液相色谱同时测定氧化型染发产品中33种禁限用染发剂含量的分析方法。采用Waters Atlantis^® T3 MV Kit色谱柱（250 mm×4.6 mm，5 μm），以磷酸盐缓冲液-乙腈为流动相，梯度洗脱，流速为1.0 mL/min，柱温为25℃；采用二极管阵列检测器（DAD），检测波长为235及280 nm，进样量为5 μL。结果表明，各成分在线性范围内线性关系良好，相关系数均高于0.999，各成分精密度实验相对标准偏差（RSDs）均小于2%；四氨基嘧啶硫酸盐和2，4-二氨基苯氧基乙醇盐酸盐在12 h内稳定性实验RSDs小于5%，其余31种成分在24 h内稳定性实验RSDs均小于5%；各成分在3个浓度水平下的加标回收率为77.6%~116.3%。该方法简便、快速、准确，适用于氧化型染发产品中多种染发剂的检测。     

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

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^-1L-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...     

高效液相色谱法测定氧化型染发产品中40种染发剂

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 Atlantis^® T3 MV Kit色谱柱(250 mm×4.6 mm, 5 μm)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5~168 μg/g,定量限为16~504 μg/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。     

Determination of hydroxypropyl bis (N-hydroxyethyl-p-phenylenediamine) hydrochloride in hair dye products by HPLC and its verification by LC-MS/MSEI北大核心CSCD

A method for the determination of hydroxypropyl bis (N-hydroxyethyl-p-phenylenediamine)hydrochloride in hair dye products by high performance liquid chromatography (HPLC) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed. The sample was ultrasonically extracted with 50% (V/V) ethanol. Chromatographic separation was carried out on a Waters Symmetry C18 column (250 mm×4.6 mm, 5 µm) by isocratic elution. The mobile phase was 0.02 mol/L ammonium acetate aqueous solution and acetonitrile (84∶16, V/V). The detection wavelength was 258 nm. Quantification was performed by external standard method. Verification for positive samples was performed by LC-MS/MS. The results showed good linearity from 2 mg/L to 200 mg/L, with the correlation coefficients (r) higher than 0.999. The limit of detection (LOD) was 0.003%(w/w), and the limit of quantification (LOQ) was 0.01%(w/w). The average spiked recoveries at three levels in both cream and liquid substrates were from 97.5% to 103.4%, with the relative standard deviations (RSDs) from 1.7% to 3.9%. The method could be used to detect hydroxypropyl bis (N[1]hydroxyethyl-p-phenylenediamine)hydrochloride in hair dye products, which could fill the gap of the current standard. © 2023, Youke Publishing Co.,Ltd. All rights reserved.