高效液相色谱法测定洗发护发产品中18种防腐剂和去屑剂  

Determination of 18 preservatives and anti-dandruff agents in shampoo and hair care products by HPLC

作　　者：祝壮飞[1] 徐勤科 刘婷媛 孙莺 雷虹 Zhuangfei Zhu;Qinke Xu;Tingyuan Liu;Ying Sun;Hong Lei(National Institutes for Food and Drug Control,Beijing 102629,China;Gansu Institute for Drug Control,Lanzhou,Gansu 730000,China)

机构地区：[1]中国食品药品检定研究院,北京102629 [2]甘肃省药品检验研究院,甘肃兰州730000

出　　处：《日用化学工业（中英文）》2024年第4期477-483,共7页China Surfactant Detergent & Cosmetics

基　　金：甘肃省药品监督管理局项目(2022GSMPA0025);甘肃省药品监督管理局项目(2020GSMPA010);甘肃省药品监督管理局项目(2021GSMPA0014);甘肃省科技厅项目(22YF7FA080)。

摘　　要：建立高效液相色谱法(HPLC)同时测定不同基质化妆品中18种防腐剂和去屑剂组分的含量,并对50批市售洗发护发类化妆品进行质量分析。不同基质样品经前处理提取后,采用HPLC法分析,外标法定量。选取C18色谱柱(4.6 mm×250 mm,5μm),甲醇和磷酸二氢钠水溶液(pH调节至3.8)作为流动相,进行梯度洗脱,流速为1.0 mL/min,柱温30℃,选取二极管阵列检测器多波长分析。18种组分在色谱图中分离度良好,峰面积与质量浓度在0.4~600μg/mL范围内呈良好的线性关系(r>0.9983),检出浓度在0.4~10 mg/kg之间。多种组分平均回收率(n=6)为83.1%~110.4%,RSD为0.12%~7.6%,回收率良好;多种组分在24 h内保持稳定,RSD在0.15%~3.8%之间,稳定性良好。50批样品中检出9种成分,吡硫鎓锌、吡罗克酮乙醇胺盐、对氯间甲酚、氯咪巴唑、三氯生、水杨酸的含量分别为2100~6800,39~2900,130~370,24~1600,0.14~0.19,28~1900 mg/kg。苄氯酚、邻氨基苯酚、邻伞花烃-5-醇的含量检出但是含量小于定量限,无法准确定量。该方法经方法学验证,可同时测定化妆品中18种防腐剂和去屑剂组分的含量。A high performance liquid chromatography(HPLC)method for simultaneous determination of 18 preservatives and anti-dandruff components in cosmetics of different bases was established,and the quality of 50 batches of commercially available shampoo and hair care cosmetics was analyzed.After the extraction of samples of different bases,the samples were analyzed by HPLC and quantified by external standard method.A C18 column(4.6 mm×250 mm,5μm)was used and an aqueous mixture of methanol and sodium dihydrogen phosphate(pH adjusted to 3.8)was selected as mobile phase for gradient elution.The flow rate was 1.0 mL/min.The column temperature was 30℃.The chromatographic separation of the 18 components was good.The linearity between peak area and mass concentration was good(r>0.9983)in the range of 0.4-600μg/mL,and the detection limit was 0.4-10 mg/kg.The average recoveries(n=6)were 83.1%-110.4%,the RSDs were 0.12%-7.6%,and the recoveries were good.These components remained stable within 24 h with RSDs ranging from 0.15% to 3.8%,indicative of good stability.Nine components were detected in 50 batches of samples,including pyrithione zinc,piroctone olamine,p-chloro-m-cresol,climbazole,triclosan and salicylic acid,whose content was 2100-6800,39-2900,130-370,24-1600,0.14-0.19,28-1900 mg/kg,respectively.Benzyl chlorophenol,o-aminophenol and o-cymen-5-ol were detected,but their content was less than the limit of quantitation and thus could not be accurately quantified.Therefore,this method could be used to simultaneously determine the 18 antiseptic and anti-dandruff components in cosmetics.

关 键 词：防腐剂 去屑剂 高效液相色谱 含量测定 

分 类 号：TQ658[化学工程—精细化工]