摘要
目的建立决明降脂灵咀嚼片的质量标准及微生物限度检查方法。方法采用TLC法,对决明降脂灵咀嚼片中的决明子药材进行定性鉴别;采用《中国药典》2015年版微生物限度检查法对决明降脂灵咀嚼片进行验证实验,并对3批样品进行微生物限度检查;建立HPLC法同时测定决明降脂灵咀嚼片中决明子的有效成分大黄酚和橙黄决明素。色谱柱为WelchromC18(200mm×4.6mm,5μm);流动相为乙腈-1mL·L^-1磷酸溶液,梯度洗脱(0~15min40∶60,15~30min40∶60~90∶10,30~40min90∶10,40~60min90∶10~40∶60),检测波长为284nm,进样量为10μL,流速为1.0mL·min^-1,柱温为30℃。结果决明子药材的TLC特征斑点清晰,分离度好,阴性无干扰,专属性较好。3批决明降脂灵咀嚼片微生物计数法适用性实验中,需氧菌总数、霉菌和酵母菌总数各菌的回收率均在50%~200%范围内,且均未检出大肠埃希菌,验证组可检出大肠埃希菌,证明该验证方法可行。在选定的色谱条件下,大黄酚和橙黄决明素具有良好的分离度和稳定性;大黄酚在0.204~10.200μg·mL^-1范围内线性关系良好,回归方程为y1=86740x1+2179.8,r1=0.9999,平均加样回收率为100.15%,RSD值为2.51%(n=6);橙黄决明素在2~80μg·mL-1范围内线性关系良好,回归方程为y2=77682x2+17104,r2=1.0000,平均加样回收率为99.00%,RSD值为1.17%(n=6)。结论实验所采用的定性、定量及微生物限度检查方法简便,专属性强,结果准确可靠,可作为决明降脂灵咀嚼片的质量控制标准及微生物限度检查方法。
Objective To establish a quality standard and microbial limit test for Jueming Jiangzhiling Chewable Tablets.Methods TLC method of qualitative identification was used to identify Cassiae semen in Jueming Jiangzhiling Chewable Tablets.The microbial limit test method validation was conducted according to Chinese Pharmacopoeia(2015 edition).3 batches of Jueming Jiangzhiling Chewable Tablets were tested by using the validated method.The content of chrysophanol and aurantio-obtusin were determined by HPLC.The HPLC method was adopted on a Welchrom C 18(200 mm×4.6 mm,5μm)column with the mobile phase of acetonitrile-1 mL·L^-1 phosphonic acid with gradient elution(0-15 min 40∶60,15-30 min 40∶60-90∶10,30-40 min 90∶10,40-60 min 90∶10-40∶60)at a flow rate of 1.0 mL·min^-1.The detection wavelength was 284 nm,the column temperature was 30℃and the injection volume was 10μL.Results The TLC spots of Cassia semen were clear with good resolution and without any interference of negative samples.The recoveries of each validation strain for the total aerobic micribial count,total yeasts and mold count were among 50%-200%,and Escherichia coli was not detected.Escherichia coli could be tested by using this validation method.The HPLC experiment results showed a good linearity within the range of 0.204-10.200μg·mL^-1 for chrysophanol,linear regression equation was y 1=86 740 x 1+2 179.8(r 1=0.999 9),the average recovery was 100.15%with RSD 2.51%(n=6).The results showed a good linearity within the range of 2-80μg·mL^-1 for aurantio-obtusin,with linear regression equation was y2=77 682x2+17 104(r2=1.000 0),the average recovery was 99.00%with RSD 1.17%(n=6).Conclusion The method is simple,accurate and reproducible.It can be used as the quality control method and microbial limit test of Jueming Jiangzhiling Chewable Tablets.
作者
吴琼
姚东
胡北
崔亚玲
王芳
何静
马宏达
WU Qiong;YAO Dong;HU Bei;CUI Yaling;WANG Fang;HE Jing;MA Hongda(Department of Pharmacy,General Hospital of Northern Theater Command,Shenyang 110016,China)
出处
《西北药学杂志》
CAS
2019年第4期452-457,共6页
Northwest Pharmaceutical Journal
基金
军队医疗机构制剂标准提高科研专项重点课题(编号:13ZJZ02)
