反相-高效液相色谱法测定软膏剂中葡萄糖酸氯己定含量  

Quantitative determination of Chlorhexidine Gluconate in ointments by reversed-phase high performance liquid chromatography

作　　者：孙晶晶[1] 杨旭 宁科权 岂蕊 SUN Jingjing;YANG Xu;NING Kequan;QI Rui(Chemical Room,Jilin Provincial Institute for Drug Control,Jilin Province,Changchun130033,China;Chemical Room,Meihekou Food and Drug Inspection and Testing Center,Jilin Province,Meihekou135000,China)

机构地区：[1]吉林省药品检验所化学室,吉林长春130033 [2]吉林省梅河口市食品药品检验检测中心化学室,吉林梅河口135000

出　　处：《中国当代医药》2023年第10期26-29,共4页China Modern Medicine

摘　　要：目的采用反相-高效液相色谱法测定葡萄糖酸氯己定软膏中葡萄糖酸氯己定的含量。方法采用资生堂CAPCELLPAK C_(18)MGⅡ(250 mm×4.6 mm,5μm)色谱柱,以乙腈-磷酸盐溶液(磷酸调pH至3.0)为流动相,梯度洗脱,流速1.0 ml/min,检测波长为239 nm,柱温为30℃。结果在8.044~64.352μg/ml范围内线性关系良好(r=0.999996);四家企业样品的平均回收率(n=9)分别为100.5%、100.5%、98.7%、100.0%,RSD分别为0.5%、0.5%、0.7%、0.1%;仪器精密度实验,连续6针峰面积的RSD为0.5%;按照信噪比10∶1计算,葡萄糖氯己定定量限为0.58μg;稳定性实验,24 h内峰面积的RSD为0.5%;重复性实验,测定6份样品含量的RSD为1.3%。结论该方法可消除基质对测定结果的影响,专属性强、重复性好,有利于更好地控制该药品质量。Objective To determine the content of Chlorhexidine Gluconate in Chlorhexidine Gluconate Ointment by reversed-phase high performance liquid chromatography.Methods Shiseido CAPCELLPAK C_(18)MGⅡ(250 mm×4.6 mm,5μm)column was used,and the acetonitrile-phosphate solution(adjusted to pH 3.0 with phosphoric acid)was used as the mobile phase,and the gradient elution was obtained at a flow rate of 1.0 ml/min,the detection wavelength was 239 nm,and the column temperature was 30℃.Results The linear relationship was good in the range of 8.044-64.352μg/ml(r=0.999996),and the average recovery rate(n=9)of the samples of the four enterprises was 100.5%,100.5%,98.7%,and 100.0%,and the RSD was 0.5%,0.5%,0.7%,and 0.1%,respectively.Instrument precision experiment,RSD of continuous 6-pin peak area was 0.5%.According to the signal-to-noise ratio of 10∶1,the quantitative limit of glucose chloride has been determined to be 0.58μg.Stability experiment,the RSD of the peak area was 0.5%within 24 hours.Reproducible experiment with 1.3%RSD for determination of 6 samples.Conclusion This method can eliminate the influence of matrix on the determination results,with strong specificity and good repeatability,which is conducive to better control of the quality of the drug.

关 键 词：软膏剂 葡萄糖酸氯己定 高效液相色谱法 含量测定 标准提高 

分 类 号：R927.2[医药卫生—药学]