离子排斥色谱法测定药用软膏及乳膏中硼酸及硼砂的含量  

Determination of boric acid and borax in ointment and cream drugs by ion exclusion chromatography

作　　者：于海英 牛水蛟 李俊婕 张良雨 李启艳 李军 YU Hai-ying;NIU Shui-jiao;LI Jun-jie;ZHANG Liang-yu;LI Qi-yan;LI Jun(Shandong Institute for Food and Drug Control/NMPA Key Laboratory for Quality Control of Cosmetics Raw Material,Jinan 250101,China)

机构地区：[1]山东省食品药品检验研究院/国家药监局化妆品原料质量控制重点实验室,济南250101

出　　处：《药物分析杂志》2022年第7期1209-1215,共7页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立采用离子排斥色谱法测定药用软膏及乳膏中硼酸及硼砂含量的方法。方法:样品经90%甲醇溶液分散提取,Cleanert IC-RP小柱净化后,以3.0 mmol·L^(-1)甲烷磺酸+60 mmol·L^(-1)甘露醇的溶液为淋洗液,25 mmol·L^(-1)四甲基氢氧化铵+15 mmol·L^(-1)甘露醇的溶液为再生液,经IonPac ICE Borate离子排斥分析柱(250 mm×9 mm)分离,抑制型电导器检测器检测。结果:硼酸质量浓度在1~200 mg·L^(-1)范围内线性关系良好,相关系数为0.999 6;检测限为0.5 mg·L^(-1),定量限为1.0 mg·L^(-1);软膏剂3个水平的加样回收率(n=3)在99.5%~99.7%,RSD在0.9%~1.3%,乳膏剂3个水平的加样回收率(n=3)在99.2%~100.2%,RSD在1.1%~1.7%。按本法对10批软膏及乳膏中的硼酸进行测定,其中5批硼酸软膏的含量为4.89%~5.21%,5批丁硼乳膏的含量为2.39%~2.68%。结论:该方法适用于软膏及乳膏中硼酸及硼砂的含量测定。Objective: To establish a method for the content determination of boric acid and borax in ointment and cream drugs by ion exclusion chromatography. Methods: The samples were dispersed and extracted by 90% methnol solution, purified by Cleanert IC-RP column, the solution of 3.0 mmol·L^(-1)methanesulfonic acid and 60 mmol·L^(-1)mannitol were used as eluent, and the solution of 25 mmol·L^(-1)tetramethylammonium hydroxide and 15 mmol·L^(-1)mannitol were used as regenerant. IonPac ICE Borate ion exclusion column(250 mm×9 mm) was used for separation and suppressor conductance was used for detection. Results: The calibration curves had good linearity within 1-200 mg·L^(-1)for the mass concentration of boric acid, r=0.999 6. The limit of detection was 0.5 mg·L^(-1)and the limit of quantitation was 1.0 mg·L^(-1). The recovery rates(n=3) of the three levels of ointment were 99.5%-99.7%, RSD were 0.9%-1.3%, and the recovery rates(n=3) of the three levels ofcream were 99.2%-100.2%, RSD were 1.1%-1.7%.The boric acid in 10 batches of ointment and cream was determined according to this method.The content of five batches of boric acid ointment was 4.89%-5.21%, and the content of five batches of boron butyrate cream was 2.39%-2.68%. Conclusion: This method is suitable for the determination of boric acid and borax in ointment and cream drugs.

关 键 词：离子排斥色谱 消毒防腐药 软膏 乳膏 硼酸 硼砂 含量测定 

分 类 号：R917[医药卫生—药物分析学]