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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10 μL。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、5.02~250.82 μg/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、0.15 μg/mL;定量限分别为0.84、0.36、1.29、0.41、0.65、0.78、0.33、0.50 μg/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 were 0.84, 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.
高效液相色谱-二极管阵列检测器法血脂康胶囊他汀类异黄酮类含量测定
HPLC-DADXuezhikang capsulesStatinsIsoflavonesContent determination
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