超高效液相色谱法同时测定障眼明胶囊中7个成分的含量

Simultaneous Determination of Seven Components in Zhangyanming Capsules by UPLC

目的建立超高效液相色谱法(UPLC)同时测定障眼明胶囊中7个成分含量的方法。方法采用Waters Acquity UPLC BEH C18柱(2.1 mm×100 mm,1.8μm)色谱柱,乙腈(A)-0.5%醋酸水溶液(B)为流动相,梯度洗脱;流速0.3 ml/min,柱温30℃,检测波长分别为230 nm(检测芍药苷和京尼平苷酸)、250 nm(检测葛根素)、330 nm(检测毛蕊花糖苷)、360 nm(检测金丝桃苷)、284 nm(检测橙黄决明素和大黄酚),进样量:2μl。结果橙黄决明素、大黄酚、毛蕊花糖苷、京尼平苷酸、金丝桃苷、葛根素、芍药苷的线性范围分别为4.008~24.04μg/ml(r=0.9998),3.101~18.61μg/ml(r=0.9996),1.266~7.601μg/ml(r=0.9997),2.519~15.12μg/ml(r=0.9995),2.238~13.43μg/ml(r=0.9993),1.603~9.619μg/ml(r=0.9994),0.8864~5.318μg/ml(r=0.9992),平均加样回收率(n=6)为98.03%~101.27%,RSD为0.657%~1.08%。障眼明胶囊中橙黄决明素、大黄酚、毛蕊花糖苷、京尼平苷酸、金丝桃苷、葛根素、芍药苷7个成分的含量范围分别为:0.5984~0.6235 mg/g,0.3866~0.3952 mg/g,0.0855~0.0879 mg/g,0.1279~0.1411 mg/g,0.0911~0.0933 mg/g,0.3002~0.3186 mg/g,0.1021~0.1109 mg/g。结论该本法准确性高、快速高效,可用于障眼明胶囊的质量控制。

Objective To establish an UPLC method for simultaneous determination of seven constituents in Zhangyanming Capsules. Methods The analysis was performed on a Waters Acquity UPLC BEH C18(2.1 mm×100 mm, 1.8 μm)chromatographic column. The column temperature was set at 30 °C and the sample size was 2 μl. The mobile phase of gradient elution was acetonitrile(A)-0.5 % acetic acid(B) at the flow rate of 0.3 ml/min. The detection wavelength were set at 230 nm(for determination of paeoniflorin and geniposidic acid), 250 nm(for determination of puerarin),330 nm(for determination of verbascoside), 360 nm(for determination of hyperoside) and 284 nm(for determination of aurantio-obtusin and chrysophanol). The injection volume of samples was 2 μl. Results The linear ranges of aurantio-obtusin, chrysophanol, verbascoside, geniposidic acid, hyperoside, puerarin and paeoniflorin were 4.008-24.04 μg/ml(r=0.9998), 3.101-18.61 μg/ml(r=0.9996), 1.266-7.601 μg/ml(r=0.9978), 2.519-15.12 μg/ml(r=0.9995), 2.238-13.43 μg/ml(r=0.9993), 1.603-9.619 μg/ml(r=0.994) and 0.8864-5.318 μg/ml(r=0.9992),respectively. The mean recoveries(n=6) were in the range of 98.03 %-101.27 %, with RSDs of 0.657 %-1.08 %. The contents of aurantio-obtusin, chrysophanol, verbascoside, geniposidic acid, hyperoside, puerarin and paeoniflorin in Zhangyanming Capsules were 0.5984-0.6235, 0.3866-0.3952, 0.0855-0.0879, 0.1279-0.1411, 0.0911-0.0933, 3002-0.3186, 0.1021-0.1109 mg/g, respectively. Conclusion The established UPLC method is accurate, fast and highly efficient, which can be used to determine seven constituents in Zhangyanming Capsules.