高效液相色谱法同时测定化妆品中8种防腐剂  

Determination of Eight Kinds of Preservatives in Cosmetics by HPLC

作　　者：陈静[1] 毛北萍[1] 袁晓倩 韩晶[1] 郑荣[1] CHEN Jing;MAO Beiping;YUAN Xiaoqian;HAN Jing;ZHENG Rong(Shanghai Institute of Food and Drug Control,Shanghai 201203,China)

机构地区：[1]上海市食品药品检验所,上海201203

出　　处：《香料香精化妆品》2020年第5期40-45,共6页Flavour Fragrance Cosmetics

摘　　要：建立了同时测定化妆品中8种防腐剂的高效液相色谱方法。对不同基质类型的化妆品样品加入溶剂超声提取,提取液经高速离心处理,上清液以正己烷脱脂,经0.22μm微孔滤膜过滤后取续滤液,色谱柱为Exmere Avanti BDS Quattro (4.6 mm×250 mm×5μm),流动相为质量分数0.1%三氟乙酸水溶液-乙腈,梯度洗脱,流速为1.0 m L/min,柱温为30℃,进样量10μL,经高效液相色谱-二极管阵列检测器测定,外标法定量。结果发现,8种防腐剂在一定浓度范围内呈良好线性关系(相关系数均大于0.9999);回收率(n=6)在88.0%~120.1%,相对标准偏差小于6.9%,化合物十二烷基三甲基溴化铵(DTAC)的最低检出质量比为150μg/g,化合物吡硫鎓锌、己脒定、氯己定的最低检出质量比为10μg/g,其余化合物的最低检出质量比为40μg/g。该方法灵敏度高,重复性好,操作简单,填补了《化妆品安全技术规范》(2015年版)中的监管空白,有利于规范化妆品行业对该类防腐剂的使用。A HPLC method for the simultaneous determination of eight kinds of preservatives in cosmetics was established.Different forms of cosmetic samples were treated by ultrasonic extraction,the extraction solution was obtained by high-speed centrifugation,the supernatant was degreased by hexane,and then filtered by 0.22μm millipore filter,finally the continued filtrate was taken for analysis.A Waters reversed phase column,Exmere Avanti BDS Quattro(4.6 mm×250 mm×5μm)was used with 0.1%(mass fraction)trifluoroacetic acid in aqueous-acetonitrile as the mobile phase under the condition of gradient elution.When the flow rate was 1.0 mL/min,column temperature was 30℃,the injection volume was 10μL,the samples were determined by high performance liquid chromatography-diode array detector,and quantified by external standard method.The results showed that the recoveries(n=6)were 88.0%to 120.1%,relative standard deviation was blow 6.9%,detection limit of DTAC was 150μg/g,detection limits of zinc pyrithione,hexamidine and chlorhexidine were 10μg/g,detection limits of the rest compounds were 40μg/g.The method has advantages of high sensitivity,good reproducibility,easy operation,which filled the blanks of Safety and Technical Standards for Cosmetics(2015 edition),and it can be used to determine the content of preservatives in cosmetics and is beneficial to regulate the use of such preservatives in cosmetics industry.

关 键 词：化妆品 高效液相色谱法 防腐剂 苯扎氯铵 苄索氯铵 吡硫鎓锌 己脒定 氯己定 

分 类 号：O657.72[理学—分析化学] TQ658[理学—化学]