摘要
目的建立同时测定联苯苄唑乳膏中8种抑菌剂和1种抗氧剂含量的方法。方法采用CAPCELL PAK ADME色谱柱,以0.02 mol/L乙酸铵溶液-甲醇为流动相,梯度洗脱,体积流量为1.0 mL/min,柱温为30℃,检测波长为218 nm。进行专属性、线性关系、检测限与定量限、精密度、回收率、稳定性等方法学考察。检测来自13家生产企业、共37批次联苯苄唑乳膏中抑菌剂山梨酸、苯甲酸、苯甲醇、尼泊金甲酯、尼泊金乙酯、尼泊金丙酯、尼泊金丁酯、苯扎溴铵和抗氧剂二丁基羟基甲苯(BHT)的含量。结果抑菌剂山梨酸、苯甲酸、苯甲醇、尼泊金甲酯、尼泊金乙酯、尼泊金丙酯、尼泊金丁酯、苯扎溴铵和抗氧剂BHT的线性范围分别为9.924~198.5、10.43~208.6、24.94~498.7、10.07~201.5、10.13~202.6、10.13~202.5、10.03~200.5、4.053~81.04、10.10~202.0μg/mL(r为0.9993~1.0000);平均回收率为98.6%~100.9%(RSD为0.52%~1.43%)。专属性、检测限与定量限、精密度、稳定性等方法学考察均符合要求。各批次苯苄唑乳膏均未检出苯甲酸、尼泊金甲酯、尼泊金丙酯和尼泊金丁酯,检出山梨酸、苯甲醇、尼泊金乙酯、苯扎溴铵和BHT。结论建立的方法操作简便、结果准确,可用于联苯苄唑乳膏中抑菌剂和抗氧剂含量的同时测定。
Objective To establish a method for simultaneous determination of eight bacteriostats and one antioxygen in Bifonazole Cream.Methods The determination was performed on CAPCELL PAK ADME column with mobile phase consisted of 0.02 mol/L ammonium acetate solution-methanol in gradient elution at a flow rate of 1.0 mL/min.The column temperature was 30℃,and detection wavelength was set at 218 nm.The specificity,linear relationship,limit of detection and limit of quantitation,precision,recovery,stability were investigated.The contents of sorbic acid,benzoic acid,benzyl alcohol,methyl paraben,ethyl paraben,propyl paraben,butyl paraben,benzalkonium bromide and antioxidant dibutyl hydroxytoluene(BHT)in 37 batches of Bifonazole Cream from 13 manufacturers were determined.Results The linear range of bacteriostats sorbic acid,benzoic acid,benzyl alcohol,methylparaben,ethylparaben,propylparaben,butylparaben,benzalkonium bromide and antioxygen BHT were 9.924—198.5,10.43—208.6,24.94—498.7,10.07—201.5,10.13—202.6,10.13—202.5,10.03—200.5,4.053—81.04,10.10—202.0μg/mL(r=0.9993—1.0000)respectively.The average recoveries were 98.6%—100.9%with the RSDs of 0.52%—1.43%.The specificity,limit of detection and limit of quantification,precision,stability and other methodological investigation met the requirements.Benzoic acid,methyl paraben,propyl paraben and butyl paraben were not detected in all batches of benzimidazole cream,but sorbic acid,benzyl alcohol,ethyl Paraben,benzalkonium bromide and BHT were detected.Conclusions The method is simple and accurate,and can be used for simultaneous determination of bacteriostats and antioxygen in Bifonazole Cream.
作者
唐立超
郑淑凤
顾立强
黄剑英
李玲玲
TANG Lichao;ZHENG Shufeng;GU Liqiang;HUANG Jianying;LI Lingling(Xiamen Institution for Food and Drug Quality Control,Xiamen 361012,China)
出处
《药物评价研究》
CAS
2020年第12期2439-2443,共5页
Drug Evaluation Research
