HPLC法梯度洗脱同时测定曲安奈德益康唑乳膏中4种抑菌剂的含量  

Simultaneous determination of 4 bacteriostatic agents in triamcinolon acetonide econazole cream by HPLC under gradient elution

作　　者：李震 刘明鹭 栾曾惠 于玮洁 杨钊 LI Zhen;LIU Minglu;LUAN Zenghui;YU Weijie;YANG Zhao(Qingdao Institute for Food and Drug Control,Qingdao 261000,China;Qingdao Women and Children′s Hospital,Qingdao 261000,China)

机构地区：[1]青岛市食品药品检验研究院,山东青岛261000 [2]青岛妇女儿童医院,山东青岛261000

出　　处：《中国药品标准》2024年第2期204-208,共5页Drug Standards of China

摘　　要：目的:建立梯度洗脱HPLC法,以双波长同时测定不同厂家曲安奈德益康唑乳膏中4种抑菌剂含量。方法:采用Waters Symmetry C 18(250 mm×4.6 mm,5μm)色谱柱,以甲醇为流动相A,以甲醇-0.02 mol·L^(-1)磷酸二氢钠溶液(95∶5)为流动相B,梯度洗脱,流速为1.0 mL·min-1,柱温为35℃,检测波长为228 nm、254 nm。结果:本法可有效分离曲安奈德益康唑乳膏中各色谱峰,苯甲酸、羟苯甲酯、羟苯乙酯和羟苯丙酯分别在0.010348~0.15522 mg·mL^(-1)、0.009876~0.148145 mg·mL^(-1)、0.010106~0.151588 mg·mL^(-1)、0.010259~0.153882 mg·mL^(-1)范围内与峰面积线性关系良好;平均回收率(n=9)分别为99.68%(RSD=2.35%)、100.21%(RSD=1.78%)、100.47%(RSD=1.59%)、100.06%(RSD=1.65%),检测限分别为3×10^(-5)mg·mL^(-1)、1.67×10^(-5)mg·mL^(-1)、1.67×10^(-5)mg·mL^(-1)、1.67×10^(-5)mg·mL^(-1)。结论:本研究建立的曲安奈德益康唑乳膏中抑菌剂的含量测定方法,方法灵敏、准确,色谱峰分离良好,为其质量控制提供了依据。Objective:To develop an HPLC method with gradient elution for the simultaneous determination of 4 bacteriostatic agents in triamcinolone acetonide econazole cream from the different manufacturers.Methods:The test was performed on a Waters Symmetry C 18 column(250 mm×4.6 mm,5μm)under gradient elution of methanol(A)and methanol-0.02 mol·L^(-1)sodium dihydrogen phosphate solution(B).The flow rate of 1.0 mL·min-1 and the column temperature was 35℃.The detection wavelengths were 228 nm and 254 nm.Results:The good separation of the bacteriostatic agents peaks were achieved.The linear ranges of benzoic acid,methyl hydroxybenzoate,ethylparaben and propylparaben fell into 0.010348-0.15522 mg·mL^(-1),0.009876-0.148145 mg·mL^(-1),0.010106-0.151588 mg·mL^(-1)and 0.010259-0.153882 mg·mL^(-1)respectively.The average recoveries were 99.68%(RSD=2.35%),100.21%(RSD=1.78%),100.47%(RSD=1.59%)and 100.06%(RSD=1.65%)respectively.The LODs were 3×10^(-5)mg·mL^(-1),1.67×10^(-5)mg·mL^(-1),1.67×10^(-5)mg·mL^(-1)and 1.67×10^(-5)mg·mL^(-1)respectively.Conclusion:The established method is sensitive and accurate,and has the good separation.It provides the reliable basis for the quality control of triamcinolone acetonide econazole cream.

关 键 词：曲安奈德益康唑乳膏 抑菌剂 苯甲酸 羟苯甲酯 羟苯乙酯 羟苯丙酯 

分 类 号：R921.2[医药卫生—药学]