决明降脂灵咀嚼片的质量标准及微生物限度检查
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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Welchrom C18(200mm×4.6mm,5μm);流动相为乙腈~(-1)mL·L~(-1)磷酸溶液,梯度洗脱(0～15min 40∶60,15～30min 40∶60～90∶10,30～40min 90∶10,40～60min 90∶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y_1=86 740x_1+2 179.8,r_1=0.999 9,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y_2=77 682x_2+17 104,r_2=1.000 0,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 semenin Jueming Jiangzhiling Chewable Tablets.The microbial limit test method validation was conducted according to Chinese Pharmacopoeia(2015edition).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)(200mm×4.6mm,5μm)column with the mobile phase of acetonitrile-1mL·L~(-1)phosphonic acid with gradient elution(0-15min 40∶60,15-30min 40∶60-90∶10,30-40min 90∶10,40-60min 90∶10-40∶60)at a flow rate of 1.0mL·min~(-1).The detection wavelength was 284nm,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 740x_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 y_2=77 682x_2+17 104(r_2=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.
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 semenin Jueming Jiangzhiling Chewable Tablets.The microbial limit test method validation was conducted according to Chinese Pharmacopoeia(2015edition).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)(200mm×4.6mm,5μm)column with the mobile phase of acetonitrile-1mL·L~(-1)phosphonic acid with gradient elution(0-15min 40∶60,15-30min 40∶60-90∶10,30-40min 90∶10,40-60min 90∶10-40∶60)at a flow rate of 1.0mL·min~(-1).The detection wavelength was 284nm,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 740x_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 y_2=77 682x_2+17 104(r_2=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.
引文
[1]中央军委后勤保障部卫生局.中国人民解放军医疗机构制剂规范:2015年版:第一册[M].北京:人民军医出版社,2015.
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[4]崔明筠,付开聪.降脂清片薄层色谱鉴别[J].亚太传统医药,2017,13(1):29-31.
[5]张丽梅,李俊,褚阳,等.清源调脂胶囊质量标准的提高[J].中国药师,2016,19(10):1972-1975.
[6]严亚锋,白海侠,史亚军.脑清通颗粒质量标准的研究[J].西部中医药,2016,29(2):23-26.
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[8]马慧萍,葛欣,何蕾,等.润肠通便颗粒质量标准研究[J].解放军药学学报,2012,28(5):428-431.
[9]杨静,詹才智,柴建辉.2种医院制剂微生物限度检查方法的建立[J].医药导报,2017,36:79-81.
[10]何倩灵,郭峰,谭琴,等.芪贞慢咽宁颗粒微生物限度检查法的建立及方法学验证[J].海峡药学,2017,29(6):49-51.
[11]刘栋,宋晓红,王丽军,等.泽菊降脂片中橙黄决明素和大黄酚的定性鉴别和含量测定[J].中国药师,2017,20(1):163-165.
[12]刘敏,贾海红,刘彦,等.高效液相色谱法同时测定降脂灵片中4种蒽醌类成分的含量[J].河北医科大学学报,2015,36(1):52-55.
[13]张倩,吴翠,朱文灯,等.HPLC法测定五味决明茶中大黄酚和橙黄决明素的含量[J].海峡药学,2015,27(6):73-74.
[14]罗珍妹.降脂灵颗粒质量标准研究[J].海峡药学,2012,24(10):73-75.
[15]王云霞,张鑫.变换波长HPLC同时测定决明子中橙黄决明素和大黄酚的含量[J].陕西中医,2016,37(8):1080-1081.
[16]卫莹芳,谢达温,万丽,等.HPLC梯度洗脱法同时测定决明子中橙黄决明素、大黄素、大黄酚和大黄素甲醚的含量[J].世界科学技术-中医药现代化,2009,11(6):868-871.
[17]黄小平,钟国跃,张雪梅,等.HPLC法测定决明子中大黄酚和橙黄决明素[J].中国中药杂志,2010,35(16):2065-2067.
[18]崔亚玲,李昕,胡北,等.清石颗粒质量标准及微生物限度检查[J].西北药学杂志,2017,32(5):574-579.
[19]胡轶娟,万丽,张加雄,等.高效液相色谱法测定不同产地决明子中橙黄决明素含量[J].时珍国医国药,2006,17(7):1138-1139.
[20]王小凤,樊淑彦,何晓文,等.山庄降脂片中橙黄决明素、大黄素和大黄酚的HPLC测定[J].中国医药工业杂志,2009,40(10):770-772.
[2]国家药典委员会.中国药典:2015年版:一部[S].北京:中国医药科技出版社,2015:31,145
[3]国家药典委员会.中国药典:2015年版:四部[S].北京:中国医药科技出版社,2015.
[4]崔明筠,付开聪.降脂清片薄层色谱鉴别[J].亚太传统医药,2017,13(1):29-31.
[5]张丽梅,李俊,褚阳,等.清源调脂胶囊质量标准的提高[J].中国药师,2016,19(10):1972-1975.
[6]严亚锋,白海侠,史亚军.脑清通颗粒质量标准的研究[J].西部中医药,2016,29(2):23-26.
[7]许莉,李可强,赵美瑾,等.七味养生茶质量标准研究[J].亚太传统医药,2016,12(19):21-24.
[8]马慧萍,葛欣,何蕾,等.润肠通便颗粒质量标准研究[J].解放军药学学报,2012,28(5):428-431.
[9]杨静,詹才智,柴建辉.2种医院制剂微生物限度检查方法的建立[J].医药导报,2017,36:79-81.
[10]何倩灵,郭峰,谭琴,等.芪贞慢咽宁颗粒微生物限度检查法的建立及方法学验证[J].海峡药学,2017,29(6):49-51.
[11]刘栋,宋晓红,王丽军,等.泽菊降脂片中橙黄决明素和大黄酚的定性鉴别和含量测定[J].中国药师,2017,20(1):163-165.
[12]刘敏,贾海红,刘彦,等.高效液相色谱法同时测定降脂灵片中4种蒽醌类成分的含量[J].河北医科大学学报,2015,36(1):52-55.
[13]张倩,吴翠,朱文灯,等.HPLC法测定五味决明茶中大黄酚和橙黄决明素的含量[J].海峡药学,2015,27(6):73-74.
[14]罗珍妹.降脂灵颗粒质量标准研究[J].海峡药学,2012,24(10):73-75.
[15]王云霞,张鑫.变换波长HPLC同时测定决明子中橙黄决明素和大黄酚的含量[J].陕西中医,2016,37(8):1080-1081.
[16]卫莹芳,谢达温,万丽,等.HPLC梯度洗脱法同时测定决明子中橙黄决明素、大黄素、大黄酚和大黄素甲醚的含量[J].世界科学技术-中医药现代化,2009,11(6):868-871.
[17]黄小平,钟国跃,张雪梅,等.HPLC法测定决明子中大黄酚和橙黄决明素[J].中国中药杂志,2010,35(16):2065-2067.
[18]崔亚玲,李昕,胡北,等.清石颗粒质量标准及微生物限度检查[J].西北药学杂志,2017,32(5):574-579.
[19]胡轶娟,万丽,张加雄,等.高效液相色谱法测定不同产地决明子中橙黄决明素含量[J].时珍国医国药,2006,17(7):1138-1139.
[20]王小凤,樊淑彦,何晓文,等.山庄降脂片中橙黄决明素、大黄素和大黄酚的HPLC测定[J].中国医药工业杂志,2009,40(10):770-772.