亮菌甲素对照品标定及其注射剂含量测定方法研究  

Reference substance calibration of Armillarisin A and the content determination of its injections

作　　者：康丽洁 张圆 尹菁 石蓓佳 薛敏华 陆益红 KANG Li-jie;ZHANG Yuan;YIN Jing;SHI Bei-jia;XUE Min-hua;LU Yi-hong(Department of Pharmaceutical Analysis,Xuzhou Medical University,Xuzhou Jiangsu 221004;Jiangsu Institute for Food and Drug Control,Nanjing 210019)

机构地区：[1]徐州医科大学药物分析教研室,江苏徐州221004 [2]江苏省食品药品监督检验研究院,南京210019

出　　处：《中南药学》2020年第3期497-501,共5页Central South Pharmacy

摘　　要：目的建立亮菌甲素对照品标定方法,同时建立HPLC测定亮菌甲素注射剂含量。方法对照品标定:通过紫外光谱、红外光谱、质谱、核磁共振波谱进行结构确证,采用HPLC法进行纯度检查,以质量平衡法进行定量赋值;注射剂含量测定:采用Kromasil C18色谱柱,以0.01 mol·L^-1乙酸铵溶液(pH 4.0)-甲醇(73∶27)为流动相,流速1.0 mL·min^-1,柱温40℃,检测波长367 nm。结果确证了亮菌甲素对照品的结构,测得其含量为99.6%;新建含量测定方法专属性良好,亮菌甲素浓度在8.07~80.70μg·mL^-1与峰面积线性关系良好(r=0.9999),注射用亮菌甲素(包括处方Ⅰ、处方Ⅱ)和亮菌甲素注射液平均加样回收率均在98.0%~101.0%内。24批样品含量测定结果为94.7%~102.6%,利用SPSS软件进行统计分析,结果表明,建立的HPLC法与现行标准中紫外吸收系数法含量测定结果相关性良好且差异无统计学意义。结论亮菌甲素对照品定量赋值结果准确、可靠,可作为含量测定用对照品;建立的含量测定HPLC法专属性好,准确度高,可替代原方法用于亮菌甲素注射剂的含量测定。Objective To establish a calibration method for Armillarisin A and to establish a high performance liquid chromatography method(HPLC) for the content determination of Armillarisin A injections. Methods The calibration method of reference substances was as follows: the structure was characterized by ultraviolet-visible spectrum, infrared spectrum, mass spectrum and nuclear magnetic resonance;the chromatographic purity was determined by HPLC and the quantitative value was assigned by mass balance method. The Kromasil C18 column was used with the mobile phase consisted of 0.01 mol·L^-1 ammonium acetate solution(pH 4.0)-methanol(73∶27). The flow rate was 1.0 mL·min^-1, the column temperature was maintained at 40℃ and the detection wavelength was 367 nm. Results The structure of the reference substance of Armillarisin A was confirmed and its content was 99.6%. The new content determination method showed good specificity. The linearity of Armillarisin A was at 8.07-80.70 μg·m L^-1(r = 0.9999). The average recoveries of Armillarisin A for injection(prescriptionⅠand prescriptionⅡ) and Armillarisin A injection were between 98.0%-101.0%. The content of 24 batches of samples ranged from 94.7% to 102.6%. SPSS software was used for the statistical analysis. The method had a good correlation with the UV absorption coefficient method for the determination of Armillarisin A with current standards, and there was no significant difference. Conclusion The quantitative evaluation of Armillarisin A reference is accurate and reliable, and can be used as a reference substance in the content determination. The method has good specificity, and accuracy, which can be used as an alternative to the original method for the content determination of Armillarisin A injections.

关 键 词：亮菌甲素 对照品标定 质量平衡法 

分 类 号：R927[医药卫生—药学] R917