| 吴坤林,沈秋莲,黄燕鹏,等.复方银唑散的含量测定及微生物限度检查方法学验证[J].安徽医药,2024,28(8):1532-1536. |
| 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 |
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| DOI：10.3969/j.issn.1009-6469.2024.08.010 |
| 中文关键词: 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 |
| 英文关键词: Silver sulfadiazine Ketoconazole Compound medicine Quality control High performance liquid chromatogra- phy Content determination Microbial limit Medium dilution method |
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| 中文摘要: |
| 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 C18(250 mm×4.6 mm，5 μm)；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 0.029 64~0.069 15 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 0.030 54~0.071 26 g/L浓度范围下与峰面积呈良好的线性关系( r=0.999 8)磺胺嘧啶银和酮康唑的平均回收率分别101.5%(n=6，RSD=0.33%)和 98.8%(n=6，RSD=0.65%)。采用培养基稀释法，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。采用培养为，各试验， |
| 英文摘要: |
| 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.Meth- ods The chromatographic column was Agilent C18 (250 mm×4.6 mm, 5 μm). 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 meth-od was used as the counting method for the total number of aerobic bacteria, molds and yeasts, and the control bacteria test method wasverified according to the microbial limit test method microbial limit test method of the four general principles of the Chinese Pharmaco-poeia 2020 edition.Results The linear range of silver sulfadiazine was 0.029 64-0.069 15 g/L(r = 0.999 9). The linear range of keto- conazole was 0.030 54-0.071 26 g/L(r=0.999 8).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 di- lution method.Conclusions The established HPLC method is accurate and specific, and can be used to simultaneously determine thecontent 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. |
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