HPLC-DAD法同时测定肝康复水丸剂中7个成分的含量
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摘要
目的:建立同时测定肝康复水丸剂中没食子酸、栀子苷、芍药内酯苷、芍药苷、丹酚酸B、丹皮酚和丹参酮Ⅱ_A含量的方法。方法:采用高效液相色谱(HPLC)法,以二极管阵列检测器(DAD),色谱柱为Agilent ZORBAX SB-C_18;流动相A为乙腈,流动相B为0.1%磷酸溶液,梯度洗脱;流速为1.0 m L/min;检测波长为267 nm(没食子酸)、235 nm(栀子苷、芍药内酯苷、芍药苷)、286nm(丹酚酸B)、274 nm(丹皮酚)、270 nm(丹参酮Ⅱ_A);柱温为30℃;进样量为10μL。结果:没食子酸、栀子苷、芍药内酯苷、芍药苷、丹酚酸B、丹皮酚、丹参酮Ⅱ_A检测质量浓度的线性范围分别为4.09～51.17μg/mL(r=0.999 5)、8.35～104.35μg/mL(r=0.999 1)、7.78～97.25μg/mL(r=0.999 9)、7.56～94.54μg/m L(r=0.999 3)、16.70～208.80μg/mL(r=0.999 5)、3.46～43.20μg/m L(r=0.999 7)、23.13～289.10μg/mL(r=0.999 9),检测限分别为0.09、0.15、0.13、0.12、0.16、0.04、0.24μg/mL,定量限分别为0.26、0.52、0.48、0.47、0.88、0.18、0.98μg/mL,平均回收率分别为91.83%、96.11%、96.83%、95.82%、96.93%、93.95%、94.79%(n=6),精密度试验的RSD均≤1.00%(n=6),供试品溶液48 h内稳定性试验的RSD均≤0.96%(n=6),重复性试验的RSD均≤0.99%(n=6)。结论:本方法准确、可靠,可用于肝康复水丸剂中上述7个成分的含量测定。
OBJECTIVE:To establish a method for simultaneous determination of the contents of gallic acid,jasminoidin,albiflorin,paeoniflorin,danshinolic acid B,paeonol and tanshinone Ⅱ_A in Gankangfu water pill. METHODS:HPLC method with DAD was adopted. The determination was performed on Agilent ZORBAX SB-C_18 column with mobile phase A consisted of acetonitrile and mobile phase B consisted of 0.1% phosphate solution (gradient elution) at the flow rate of 1.0 mL/min. The detection wavelengths were set at 267 nm (gallic acid),235 nm (jasminoidin,albiflorin,paeoniflorin),286 nm (danshinolic acid B),274 nm (paeonol) and 270 nm (tanshinone Ⅱ_A). The column temperature was set at 30 ℃ and sample size was 10 μL.RESULTS:The linear range of gallic acid,jasminoidin,albiflorin,paeoniflorin,danshinolic acid B,paeonol and tanshinone Ⅱ_A were 4.09-51.17 μg/mL (r=0.999 5),8.35-104.35 μg/mL (r=0.999 1),7.78-97.25 μg/mL (r=0.999 9),7.56-94.54 μg/mL (r=0.999 3),16.70-208.80 μg/mL (r=0.999 5),3.46-43.20 μg/mL (r=0.999 7),23.13-289.10 μg/mL (r=0.999 9),respectively.The detection limits were 0.09,0.15,0.13,0.12,0.16,0.04 and 0.24 μg/m L;quantitative limits were 0.26,0.52,0.48,0.47,0.88,0.18 and 0.98 μg/mL,respectively. The average recovery rates were 91.83%,96.11%,96.83%,95.82%,96.93%,93.95%and 94.79%,respectively (n=6). RSDs of precision test were not more than 1.00% (n=6). RSDs of stability test were not more than 0.96% within 48 h (n=6),and RSDs of repeatability test were than 0.99%(n=6). CONCLUSIONS:The method is accurate and reliable,and can be used for content determination of above 7 components in Gankangfu water pill.
OBJECTIVE:To establish a method for simultaneous determination of the contents of gallic acid,jasminoidin,albiflorin,paeoniflorin,danshinolic acid B,paeonol and tanshinone Ⅱ_A in Gankangfu water pill. METHODS:HPLC method with DAD was adopted. The determination was performed on Agilent ZORBAX SB-C_18 column with mobile phase A consisted of acetonitrile and mobile phase B consisted of 0.1% phosphate solution (gradient elution) at the flow rate of 1.0 mL/min. The detection wavelengths were set at 267 nm (gallic acid),235 nm (jasminoidin,albiflorin,paeoniflorin),286 nm (danshinolic acid B),274 nm (paeonol) and 270 nm (tanshinone Ⅱ_A). The column temperature was set at 30 ℃ and sample size was 10 μL.RESULTS:The linear range of gallic acid,jasminoidin,albiflorin,paeoniflorin,danshinolic acid B,paeonol and tanshinone Ⅱ_A were 4.09-51.17 μg/mL (r=0.999 5),8.35-104.35 μg/mL (r=0.999 1),7.78-97.25 μg/mL (r=0.999 9),7.56-94.54 μg/mL (r=0.999 3),16.70-208.80 μg/mL (r=0.999 5),3.46-43.20 μg/mL (r=0.999 7),23.13-289.10 μg/mL (r=0.999 9),respectively.The detection limits were 0.09,0.15,0.13,0.12,0.16,0.04 and 0.24 μg/m L;quantitative limits were 0.26,0.52,0.48,0.47,0.88,0.18 and 0.98 μg/mL,respectively. The average recovery rates were 91.83%,96.11%,96.83%,95.82%,96.93%,93.95%and 94.79%,respectively (n=6). RSDs of precision test were not more than 1.00% (n=6). RSDs of stability test were not more than 0.96% within 48 h (n=6),and RSDs of repeatability test were than 0.99%(n=6). CONCLUSIONS:The method is accurate and reliable,and can be used for content determination of above 7 components in Gankangfu water pill.
引文
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[2]周军,张蕾,王杰.HPLC-DAD法测定脑血栓片中苦杏仁苷、羟基红花黄色素A、芍药苷、阿魏酸、丹酚酸B和丹参酮ⅡA[J].现代药物与临床,2015,30(3):262-266.
[3]施惠埙,童晓东,李松.HPLC-DAD法同时测定慢前康合剂中芍药苷、丹酚酸B、川续断皂苷Ⅵ、甘草酸的含量[J].中医药导报,2017,23(1):66-68.
[4]王紫燕,李春沁,穆敏婕,等.HPLC波长切换法同时测定补肾活血方中丹参素、葛根素、大豆苷和丹酚酸B的含量[J].药物分析杂志,2016,36(6):1020-1026.
[5]孙辉,何胜利.HPLC法测定心无忧片中洋川芎内酯H、洋川芎内酯I、洋川芎内酯A、藁本内酯、丹参素、丹酚酸B和丹参酮ⅡA[J].现代药物与临床,2018,33(3):464-468.
[6]杨光义,杜婷,孙荣进,等.HPLC法测定治疣胶囊中丹参酮ⅡA和丹酚酸B的含量[J].中国药师,2015,18(4):677-688.
[7]赵永明,王金,郭春燕.HPLC法同时测定丹芎通脉颗粒中5种活性成分[J].中草药,2014,45(19):2793-2796.
[8]孙殷,殷玥,刘玉梅,等.高效液相色谱-二极管阵列检测法同时测定消栓通胶囊中5种活性成分含量[J].沈阳药科大学学报,2012,29(9):702-706.
[9]李伟铭,赵月然,杨燕云,等.HPLC波长切换法同时测定白芍饮片中9个成分的含量[J].药物分析杂志,2011,31(12):2208-2212.
[10]国家药典委员会.中华人民共和国药典:一部[S].2015年版.北京:中国医药科技出版社,2015:659.
[11]张萍,杨燕,鄢丹,等.多指标成分含量测定与指纹图谱分析在中药制备工艺与质量控制中的应用[J].中华中医药杂志,2010,25(1):120-123.