HPLC-DAD法同时测定血脂康胶囊中8个成分的含量

Simultaneous Content Determination of 8 Components in Xuezhikang Capsules by HPLC-DAD

目的:建立同时测定血脂康胶囊中5个异黄酮类成分(大豆苷、染料木苷、大豆苷元、黄豆黄素和染料木素)和3个他汀类成分(洛伐他汀羟基酸、美伐他汀和洛伐他汀)含量的方法。方法:采用高效液相色谱-二极管阵列检测器法。色谱柱为Shimadzu Hypersil Gold C18;流动相为0.1%甲酸水溶液-乙腈,梯度洗脱;流速为1.0 mL/min;检测波长为256 nm(大豆苷、染料木苷、大豆苷元、黄豆黄素和染料木素)、237 nm(洛伐他汀羟基酸、美伐他汀和洛伐他汀);柱温为30℃;进样量为10μL。结果:大豆苷、染料木苷、大豆苷元、黄豆黄素、染料木素、洛伐他汀羟基酸、美伐他汀和洛伐他汀检测质量浓度的线性范围分别为5.01~250.20、3.02~150.91、2.27~113.33、3.01~150.58、3.61~180.43、4.03~201.19、3.32~166.32、5.02~250.82μg/mL(r=0.999 3~0.999 9);检测限分别为0.25、0.13、0.45、0.12、0.21、0.24、0.12、0.15μg/mL;定量限分别为0.84、0.36、1.29、0.41、0.65、0.78、0.33、0.50μg/mL;精密度、稳定性(48 h)、重复性试验的RSD均<3.0%(n=6);平均回收率分别为97.04%、98.49%、99.60%、96.14%、101.88%、96.20%、101.19%、98.46%,RSD为1.76%~4.79%(n=6)。结论:建立的方法操作简便、灵敏度高、结果准确,可用于血脂康胶囊中大豆苷、染料木苷、大豆苷元、黄豆黄素、染料木素、洛伐他汀羟基酸、美伐他汀和洛伐他汀含量的同时测定。

OBJECTIVE:To establish the method for simultaneous determination of 5 isoflavones(daidzin,genistin,daidzein,glycitein and genistein)and 3 statins(lovastatin hydroxy acid,mevastatin and lovastatin)in Xuezhikang capsules.METHODS:HPLC-DAD method was adopted.The determination was performed on Shimadzu Hypersil Gold C18 column with mobile phase consisted of 0.1% formic acid water-acetonitrile using gradient elution.The flow rate was 1.0 mL/min,and the detection wavelengths were set at 256 nm(daidzin,genistin,daidzein,glycitein and genistein)and 237 nm(lovastatin hydroxy acid,mevastatin and lovastatin).The column temperature was maintained at 30 ℃,and sample size was 10 μL.RESULTS:The linear range of daidzin,genistin,daidzein,glycitein,genistein,lovastatin hydroxy acid,mevastatin and lovastatin were 5.01-250.20,3.02-150.91,2.27-113.33,3.01-150.58,3.61-180.43,4.03-201.19,3.32-166.32,5.02-250.82 μg/mL(r=0.999 3-0.999 9),respectively.The detection limits were 0.25,0.13,0.45,0.12,0.21,0.24,0.12 and 0.15 μg/mL;the quantitation limits were0.84,0.36,1.29,0.41,0.65,0.78,0.33 and 0.50 μg/mL,respectively.RSDs of precision,stability(48 h)and reproducibility tests were all no more than 3.0%(n=6).Average recoveries were 97.04%,98.49%,99.60%,96.14%,101.88%,96.20%,101.19%,98.46%,and RSDs were 1.76-4.79%(n=6).CONCLUSIONS:The established methods is simple,sensitive,accurate,and can be applied for simultaneous content determination of daidzin,genistin,daidzein,glycitein,genistein,lovastatin hydroxy acid,mevastatin and lovastatin in Xuezhikang capsules.