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目的:建立HPLC法同时测定息喘丸中补骨脂素、佛手柑内酯、去甲蟛蜞菊内酯、蟛蜞菊内酯4个有效成分的含量。方法:采用依利特C18色谱柱(250 mm×4.6 mm,5μm);以甲醇-乙腈(2∶1)与0.5%冰醋酸溶液为流动相进行梯度洗脱;流速为1.1 ml·min-1;柱温为25℃;检测波长(0~20 min、在222 nm波长下检测补骨脂素和佛手柑内酯;20~40 min、在351 nm波长下检测去甲蟛蜞菊内酯和蟛蜞菊内酯)。结果:4个有效成分的线性范围分别为:补骨脂素5.380~107.600μg·ml-1(r=0.999 5)、佛手柑内酯6.870~137.400μg·ml-1(r=0.999 7)、去甲蟛蜞菊内酯4.580~91.600μg·ml-1(r=0.999 2)、蟛蜞菊内酯7.300~146.000μg·ml-1(r=0.999 9);平均回收率分别为96.82%、98.81%、99.06%、98.39%,RSD分别为0.77%、1.40%、1.20%、0.80%(n=6)。结论:该方法操作准确稳定、灵敏度高、重复性好,可用于息喘丸中上述4个有效成分的定量测定。
Objective: To establish an HPLC method for the simultaneous determination of psoralen, bergapten, normetholide and wedelia lactone in Xichuan pills. METHODS: Ellite C18 column (250 mm × 4.6 mm, 5 μm) was used. The mobile phase consisted of gradient elution of methanol-acetonitrile (2:1) and 0.5% acetic acid in glacial acetic acid. The flow rate was 1.1 ml · min -1. The column temperature was 25 ℃. The detection wavelength (0-20 min, detection of psoralen and bergapten at 222 nm wavelength; detection of naringlone and wedelia lactone at 351 nm for 20-40 min ). RESULTS: The linear ranges of the four active ingredients were: psoralen 5.380 ~ 107.600μg · ml-1 (r = 0.999 5), bergapten lactone 6.870 ~ 137.400μg · ml-1 (r = 0.999 7) The average recoveries of naringium lactone 4.580-91.600μg · ml-1 (r = 0.999 2) and wedelia lactone 7.300-146.000μg · ml-1 (r = 0.999 9) were 96.82%, 98.81%, 99.06 %, 98.39%, RSD 0.77%, 1.40%, 1.20%, 0.80% (n = 6) respectively. Conclusion: The method is accurate, stable, sensitive and reproducible. It can be used for the quantitative determination of the above four effective components in.