复方银唑散的含量测定及微生物限度检查方法学验证  

Methodological validation of content determination and microbial limit test of compound Yinzuo powder

作　　者：吴坤林 沈秋莲 黄燕鹏[1] 杨八十 WU Kunlin;SHEN Qiulian;HUANG Yanpeng;YANG Bashi(Department of Pharmacy,The 909th Hospital,Dongnan Hospital of Xiamen University,Zhangzhou,Fujian 363000,China)

机构地区：[1]第九〇九医院(厦门大学附属东南医院)药剂科,福建漳州363000

出　　处：《安徽医药》2024年第8期1532-1536,共5页Anhui Medical and Pharmaceutical Journal

基　　金：第九〇九医院青年苗圃课题(20YQ009)。

摘　　要：目的建立反向高效液相色谱法同时测定复方银唑散中磺胺嘧啶银和酮康唑的含量并探讨其微生物限度检查方法。方法色谱柱为Agilent C_(18)(250 mm×4.6 mm,5μm);流动相:0.07%三乙胺(A,冰醋酸调节pH至5.07)-甲醇(B),梯度洗脱:0~6 min,A80%;6~8 min,A80%~22%;8~21 min,A保持22%;21~22 min,A22%~80%,流速1.0 mL/min,检测波长:240 nm,柱温:30℃。采用培养基稀释法作为需氧菌总数、霉菌及酵母菌总数计数方法并按《中国药典》2020年版四部通则微生物限度检查法对控制菌检查法进行验证。结果磺胺嘧啶银在0.02964~0.06915 g/L浓度范围下与峰面积呈良好的线性关系(r=0.9999),酮康唑在0.03054~0.07126 g/L浓度范围下与峰面积呈良好的线性关系(r=0.9998),磺胺嘧啶银和酮康唑的平均回收率分别为101.5%(n=6,RSD=0.33%)和98.8%(n=6,RSD=0.65%)。采用培养基稀释法,各试验菌的回收率均在0.5~2.0。结论所建立的高效液相色谱法定量准确、专属性良好,可用于同时测定复方银唑散中磺胺嘧啶银和酮康唑的含量。采用培养基稀释法对复方银唑散进行微生物限度检查可行。Objective To establish a reversed-phase high performance liquid chromatography(RP-HPLC)method for simultaneous determination of silver sulfadiazine and ketoconazole in compound Yinzuo powder and to explore its microbial limit test method.Methods The chromatographic column was Agilent C_(18)(250 mm×4.6 mm,5μm).Mobile phase:0.07%triethylamine(A,pH adjusted to 5.07 with glacial acetic acid)-methanol(B),gradient elution:0-6 min,A80%;6-8 min,A80%-22%;8~21 min,A maintained 22%;21-22 min,A22%-80%,flow rate 1.0 mL/min,detection wavelength:240 nm,column temperature:30℃.The medium dilution method was used as the counting method for the total number of aerobic bacteria,molds and yeasts,and the control bacteria test method was verified according to the microbial limit test method microbial limit test method of the four general principles of the Chinese Pharmacopoeia 2020 edition.Results The linear range of silver sulfadiazine was 0.02964-0.06915 g/L(r=0.9999).The linear range of ketoconazole was 0.03054-0.07126 g/L(r=0.9998).The average recoveries of silver sulfadiazine and ketoconazole were 101.5%(n=6,RSD=0.33%)and 98.8%(n=6,RSD=0.65%),respectively.The recovery rate of each test bacteria was between 0.5 and 2.0 by medium dilution method.Conclusions The established HPLC method is accurate and specific,and can be used to simultaneously determine the content of silver sulfadiazine and ketoconazole in compound Yinzuo powder.It is feasible to carry out microbial limit test of compound Yinzuo powder by medium dilution method.

关 键 词：磺胺嘧啶银 酮康唑 复方药 质量控制 高效液相色谱法 含量测定 微生物限度 培养基稀释法 

分 类 号：R286.0[医药卫生—中药学]