HPLC法同时测定平脏调神颗粒中8种成分的含量
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摘要
目的:建立同时测定平脏调神颗粒中盐酸小檗碱、淫羊藿苷、毛蕊花糖苷、毛蕊异黄酮葡萄糖苷、芍药苷、芒果苷、丹酚酸B和葛根素含量的方法。方法:采用高效液相色谱法。色谱柱为Intert Sustain C18,流动相为乙腈-0.05 mol/L磷酸二氢钾溶液(p H为3,梯度洗脱),流速为1.0 m L/min,检测波长为250 nm(0~23 min,葛根素、芒果苷)、230 nm(>23~30 min,芍药苷)、220 nm(>30~50 min,毛蕊异黄酮葡萄糖苷、毛蕊花糖苷)、286 nm(>50~60 min,丹酚酸B)、265 nm(>60~75 min,盐酸小檗碱)、220 nm(>75~90 min,淫羊藿苷),柱温为30℃,进样量为10μL。结果:盐酸小檗碱、淫羊藿苷、毛蕊花糖苷、毛蕊异黄酮葡萄糖苷、芍药苷、芒果苷、丹酚酸B和葛根素检测质量浓度线性范围分别为4.000~400.0、4.843~484.3、0.498~49.8、2.366~236.6、23.26~2 326.0、3.067~306.7、3.629~362.9、48.23~4 823.2μg/m L(r≥0.999 4);检测限分别为0.02、0.02、0.02、0.02、0.01、0.02、0.01、0.01μg/m L,定量限分别为0.07、0.05、0.06、0.05、0.03、0.07、0.02、0.03μg/m L;精密度、稳定性(24 h)、重复性试验的RSD均<2.0%(n=6);加样回收率为95.77%~103.50%,RSD为0.77%~2.22%(n=6)。结论:建立的方法可用于平脏调神颗粒中盐酸小檗碱等8种成分含量的同时测定。
OBJECTIVE:To establish a method for simultaneous determination of berberine hydrochloride,icariin,acteoside,isoflavone glucoside,paeoniflorin,mangiferin,salvianolic acid B and puerarin in Pingzang tiaoshen granule. METHODS:HPLC method was adopted. The determination was performed on Inert Sustain C18 column with mobile phase consisted of acetonitrile-0.05 mol/L potassium dihydrogen phosphate solution(p H to 3,gradient elution)with the flow rate of 1.0 m L/min. The detection wavelength was set at 250 nm(0-23 min,puerarin,mangiferin),230 nm(>23-30 min,paeoniflorin),220 nm(>30-50 min,isoflavone glucoside,acteoside),286 nm(>50-60 min,salvianolic acid B),265 nm(>60-75 min,berberine hydrochloride),220 nm(>75-90 min,icariin). The column temperature was set at 30 ℃,and sample size was 10 μL. RESLUTS:The linear range of berberine hydrochloride,icariin,acteoside,isoflavone glucoside,paeoniflorin,mangiferin,salvianolic acid B and puerarin were 4.000-400.0,4.843-484.3,0.498-49.8,2.366-236.6,23.26-2 326.0,3.067-306.7,3.629-362.9 μ g/m L,48.23-4 823.2μg/m L(r≥0.999 4),respectively. The limits of detection were 0.02,0.02,0.02,0.02,0.01,0.02,0.01,0.01 μg/m L;the limits of quantitation were 0.07,0.05,0.06,0.05,0.03,0.07,0.02,0.03 μg/m L,respectively. RSDs of precision,stability(24 h)and repetition tests were all<2.0%(n=6). The average recoveries were 95.77%-103.50%(RSD=0.77%-2.22%,n=6). CONCLU-SIONS:Established method can be used for simultaneous determination of 8 components such as berberine hydrochloride in Pingzang tiaoshen granule.
OBJECTIVE:To establish a method for simultaneous determination of berberine hydrochloride,icariin,acteoside,isoflavone glucoside,paeoniflorin,mangiferin,salvianolic acid B and puerarin in Pingzang tiaoshen granule. METHODS:HPLC method was adopted. The determination was performed on Inert Sustain C18 column with mobile phase consisted of acetonitrile-0.05 mol/L potassium dihydrogen phosphate solution(p H to 3,gradient elution)with the flow rate of 1.0 m L/min. The detection wavelength was set at 250 nm(0-23 min,puerarin,mangiferin),230 nm(>23-30 min,paeoniflorin),220 nm(>30-50 min,isoflavone glucoside,acteoside),286 nm(>50-60 min,salvianolic acid B),265 nm(>60-75 min,berberine hydrochloride),220 nm(>75-90 min,icariin). The column temperature was set at 30 ℃,and sample size was 10 μL. RESLUTS:The linear range of berberine hydrochloride,icariin,acteoside,isoflavone glucoside,paeoniflorin,mangiferin,salvianolic acid B and puerarin were 4.000-400.0,4.843-484.3,0.498-49.8,2.366-236.6,23.26-2 326.0,3.067-306.7,3.629-362.9 μ g/m L,48.23-4 823.2μg/m L(r≥0.999 4),respectively. The limits of detection were 0.02,0.02,0.02,0.02,0.01,0.02,0.01,0.01 μg/m L;the limits of quantitation were 0.07,0.05,0.06,0.05,0.03,0.07,0.02,0.03 μg/m L,respectively. RSDs of precision,stability(24 h)and repetition tests were all<2.0%(n=6). The average recoveries were 95.77%-103.50%(RSD=0.77%-2.22%,n=6). CONCLU-SIONS:Established method can be used for simultaneous determination of 8 components such as berberine hydrochloride in Pingzang tiaoshen granule.
引文
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[12]李媛,李强.HPLC法测定感冒止咳颗粒中葛根素的含量[J].药学研究,2015,34(1):13-15.
[13]张红梅,白妮,鲁杨.高效液相色谱法同时测定土地海苓煎颗粒中芒果苷、辛弗林的含量[J].中南药学,2014,12(3):265-267.
[14]宁娜,韩建军.地骨皮的化学成分与药理作用[J].现代药物与临床,2010,25(3):172-176.
[15]杨韵,徐波.牡蛎的化学成分及其生物活性研究进展[J].中国现代中药,2015,17(12):1345-1349.
[2]时晓媞.川产黄连及其炮制品降糖化学成分与药效研究[D].成都:西南交通大学,2017:6-7.
[3]项瑞,姜丽.黄连解毒汤抗动脉粥样硬化物质基础和药理作用研究概况[J].中国药房,2016,27(4):547-549.
[4]袁航,曹树萍,陈抒云,等.淫羊藿的化学成分及质量控制研究进展[J].中草药,2014,45(24):3630-3640.
[5]卢广英,赵丽敏,许舒娅,等.基于药物体系的生地黄的质量评价研究[J].世界中医药,2015,10(5):765-771.
[6]丁慧,许纪锋,沈君子,等.黄芪中毛蕊异黄酮葡萄糖苷的含量测定[J].食品安全质量检测学报,2017,8(1):223-226.
[7]陶春,宣丽颖,林琳.赤芍的主要化学成分及药理作用研究概况[J].内蒙古民族大学学报(自然科学版),2014,29(2):198-201.
[8]孙兴欢,张宇伟,黄雪峰.知母的化学成分和药效研究进展[J].海峡药学,2015,27(3):6-12.
[9]赵国欣,刘萌,李领川,等.超高效液相色谱-质谱联用同时测定丹参中7种成分含量[J].中国实验方剂学杂志,2017,23(1):60-63.
[10]吴文杰,邓阳,谭桂林,等.一测多评法测定葛根药材中5种异黄酮类成分[J].中草药,2017,48(4):777-781.
[11]夏林丽,王协和,盛蓉.波长切换高效液相色谱法同时测定青翘抗毒颗粒中7个成分的含量[J].中国医院药学杂志,2016,36(23):2065-2070.
[12]李媛,李强.HPLC法测定感冒止咳颗粒中葛根素的含量[J].药学研究,2015,34(1):13-15.
[13]张红梅,白妮,鲁杨.高效液相色谱法同时测定土地海苓煎颗粒中芒果苷、辛弗林的含量[J].中南药学,2014,12(3):265-267.
[14]宁娜,韩建军.地骨皮的化学成分与药理作用[J].现代药物与临床,2010,25(3):172-176.
[15]杨韵,徐波.牡蛎的化学成分及其生物活性研究进展[J].中国现代中药,2015,17(12):1345-1349.