补肾祛瘀颗粒的质量标准研究
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摘要
目的:建立补肾祛瘀颗粒的质量标准。方法:采用薄层色谱(TLC)法对补肾祛瘀颗粒中的金樱子、菟丝子、制何首乌、紫草进行定性鉴别;采用紫外分光光度法测定补肾祛瘀颗粒中总多糖的含量;采用高效液相色谱(HPLC)法对补肾祛瘀颗粒中芦丁、槲皮素、金丝桃苷进行含量测定,色谱柱为BDS C_(18),流动相为乙腈-0.08%磷酸溶液(梯度洗脱),流速为1 mL/min,柱温为30℃,检测波长为370 nm,进样量为10μL。结果:4种药材的TLC供试品色谱与对照品或对照药材在相应位置上呈现相同斑点或荧光。葡萄糖、芦丁、槲皮素、金丝桃苷的检测质量浓度线性范围分别为0.003～0.018 mg/mL、0.225～7.20μg/mL、0.07～2.24μg/mL、1.25～39.88μg/mL(r=0.999 5或0.999 9,n=6),精密度、稳定性、重复性试验的RSD均≤3.80%(n=6),平均回收率分别为102.2%、101.2%、100.9%、101.0%(RSD=1.28%、2.93%、2.41%、1.59%,n=6),平均含量分别为0.46 g/g、5.48μg/g、8.18μg/g、102.88μg/g(n=3)。结论:本研究建立的补肾祛瘀颗粒的质量标准准确可靠,可为补肾祛瘀颗粒的质量控制提供科学依据。
OBJECTIVE: To establish the quality standard for Bushen quyu granules. METHODS: TLC was used for qualitative identification of Rosa laevigata,Cuscuta chinensis,processed Fallopia multiflora and Lithospermum erythrorhizon in Bushen quyu granules. And then, the content of total polysaccharides in Bushen quyu granules was determined by UV spectrophotometry. HPLC method was used for the content determination of rutin,quercetin and hyperin in Bushen quyu granules.The determination was performed on BDS C_(18) column with mobile phase consisted of acetonitrile-0.08% phosphoric acid solution(gradient elution)at the flow rate of 1 mL/min. The column temperature was 30 ℃,and detection wavelength was set at 370 nm.The sample size was 10 μL. RESULTS:TLC test sample chromatogram of 4 medicinal materials showed the same spot or fluorescence at the corresponding position with the reference substance and control medicinal materials. The linear range of glucose,rutin,quercetin and hyperin were 0.003-0.018 mg/mL,0.225-7.20 μg/m L,0.07-2.24 μg/mL and 1.25-39.88 μg/mL(r=0.999 5 or 0.999 9,n=6). RSDs of precision,stability and reproducibility tests were all less than 3%(n=6). Average recoveries were 102.2%,101.2%,100.9%,101.0%(RSD=1.28%,2.93%,2.41%,1.59%,n=6). Average contents were 0.46 g/g,5.48μg/g,8.18 μg/g and 102.88 μg/g(n=3). CONCLUSIONS:Established quality standard of Bushen quyu granules is accurate and reliable,and can provide scientific reference for quality control of Bushen quyu granules.
OBJECTIVE: To establish the quality standard for Bushen quyu granules. METHODS: TLC was used for qualitative identification of Rosa laevigata,Cuscuta chinensis,processed Fallopia multiflora and Lithospermum erythrorhizon in Bushen quyu granules. And then, the content of total polysaccharides in Bushen quyu granules was determined by UV spectrophotometry. HPLC method was used for the content determination of rutin,quercetin and hyperin in Bushen quyu granules.The determination was performed on BDS C_(18) column with mobile phase consisted of acetonitrile-0.08% phosphoric acid solution(gradient elution)at the flow rate of 1 mL/min. The column temperature was 30 ℃,and detection wavelength was set at 370 nm.The sample size was 10 μL. RESULTS:TLC test sample chromatogram of 4 medicinal materials showed the same spot or fluorescence at the corresponding position with the reference substance and control medicinal materials. The linear range of glucose,rutin,quercetin and hyperin were 0.003-0.018 mg/mL,0.225-7.20 μg/m L,0.07-2.24 μg/mL and 1.25-39.88 μg/mL(r=0.999 5 or 0.999 9,n=6). RSDs of precision,stability and reproducibility tests were all less than 3%(n=6). Average recoveries were 102.2%,101.2%,100.9%,101.0%(RSD=1.28%,2.93%,2.41%,1.59%,n=6). Average contents were 0.46 g/g,5.48μg/g,8.18 μg/g and 102.88 μg/g(n=3). CONCLUSIONS:Established quality standard of Bushen quyu granules is accurate and reliable,and can provide scientific reference for quality control of Bushen quyu granules.
引文
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[14]陈萍,万毅刚,王朝俊,等.黄蜀葵花制剂治疗慢性肾脏病的机制和疗效[J].中国中药杂志,2012,37(15):2252-2256.
[15]陈佳丽,楼婷婷,田文慧,等.正交试验法优选补肾祛瘀颗粒的提取工艺[J].中国实验方剂学杂志,2015,21(3):20-23.
[2]LI S,LIU ZH.Epidemiologic data of renal diseases from a single unit in China:analysis based on 13 519 renal biopsies[J].Kidney Int,2004,66(3):920-923.
[3]刘永芳,陈帮明,王金象,等.240例IgA肾病中医体质类型与本虚证的分布特征研究[J].中国中医药现代远程教育,2017,15(5):52-54.
[4]国家药典委员会.中华人民共和国药典:四部[S].2015年版.北京.中国医药科技出版社,2015:11,136,175,221,309,340.
[5]刘相文,侯林,崔清华,等.金樱子多糖的提取优化及其体外抗病毒活性研究[J].中药材,2017,40(7):1679-1682.
[6]张培全,谭茵,张超.菟丝子提取物清除自由基作用的研究[J].中南药学,2012,10(3):171-174.
[7]牛晓红,柏冬,宋剑南.桂枝汤水提液中总多糖含量测定[J].中国实验方剂学杂志,2013,19(13):66-68.
[8]林伟豪,陈连剑,高崇凯,等.HPLC法测定并比较茵陈蒿煎剂与配方颗粒中有效成分的含量[J].中国药房,2016,27(15):2102-2106.
[9]冯阳,陈玉梅,辛华.金樱子黄酮类成分的UPLC-Q-TOF-MS分析[J].中国实验方剂学杂志,2017,23(12):71-75.
[10]胡丽萍,王跃飞,宋殿荣,等.HPLC-UV-MS法同时测定菟丝子中5种成分的含量[J].中药材,2010,33(8):1277-1279.
[11]傅亮,楚清脆,管月清,等.中药菟丝子中生物活性成分的毛细管电泳-电化学检测[J].色谱,2005,23(5):524-527.
[12]陈清杰,杨洁,甘露珍,等.HPLC法同时测定野豌豆中芦丁、金丝桃苷、槲皮素的含量[J].中国药师,2015,18(5):861-862.
[13]冷斌.白茅根多糖对IgA肾病大鼠免疫调节及肾纤维化的干预[D].桂林:桂林医学院,2013.
[14]陈萍,万毅刚,王朝俊,等.黄蜀葵花制剂治疗慢性肾脏病的机制和疗效[J].中国中药杂志,2012,37(15):2252-2256.
[15]陈佳丽,楼婷婷,田文慧,等.正交试验法优选补肾祛瘀颗粒的提取工艺[J].中国实验方剂学杂志,2015,21(3):20-23.