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目的:建立同时测定保安万灵丹中升麻素苷、5-O-甲基维斯阿米醇苷、茅术醇、β-桉叶醇和苍术素含量的方法。方法:采用多波长HPLC梯度洗脱法:色谱柱为C18柱(200mm×4.6mm,5μm);流动相A为甲醇-乙腈(2:1),流动相B为0.1%磷酸水溶液,流速为1.0mL·min-1;进样量为20μL;检测波长分别为254nm(用于升麻素苷和5-O-甲基维斯阿米醇苷)、203nm(用于茅术醇和β-桉叶醇)和340nm(用于苍术素)。结果:升麻素苷、5-O-甲基维斯阿米醇苷、茅术醇、β-桉叶醇和苍术素的线性范围分别为4.30~86.00mg·L-1(r=0.9994)、5.85~117.00mg·L-1(r=0.9997)、16.42~328.40mg·L-1(r=0.9993)、15.16~303.20mg·L-1(r=0.9999)和12.78~255.60mg·L-1(r=0.9995);精密度、重复性及稳定性试验中所测各目标组分峰面积的RSD均小于2.0%;升麻素苷、5-O-甲基维斯阿米醇苷、茅术醇、β-桉叶醇和苍术素的平均加样回收率/RSD(n=6)分别为97.49%/1.45%、96.81%/0.94%、98.60%/1.65%、97.96%/1.38%和99.22%/1.24%。结论:本法操作简便、结果准确、重复性好,可用作保安万灵丹的质量控制方法。
OBJECTIVE: To establish a method for the simultaneous determination of cortisol, 5-O-methylvishisuvinide, methotrexate, β-eucalyptol, Methods: Multi-wavelength HPLC gradient elution was performed on a C18 column (200 mm × 4.6 mm, 5 μm). The mobile phase A was methanol-acetonitrile (2: 1) and the mobile phase B was 0.1% phosphoric acid mL · min-1; the injection volume was 20μL; the detection wavelength was 254nm for cedrolin and 5-O-methylvishweinolide respectively; 203nm for methotrexate and β- Alcohol) and 340 nm (for atractate). Results: The linear ranges of ciclinoid, 5-O-methylvishisainin, methotrexate, β-eucalyptol and atractylodes were 4.30-86.00 mg · L -1 (r = 0.9994) 5.85-117.00 mg · L -1 (r = 0.9997), 16.42-328.40 mg · L -1 (r = 0.9993), 15.16-303.20 mg · L -1 (r = 0.9999) and 12.78-255.60 mg · L -1 (r = 0.9995). The RSDs of peak area of each target component in the precision, repeatability and stability test were all less than 2.0%. Crests, 5-O-methylvishisainin, The average recoveries of RSD / RSD (n = 6) were 97.49% / 1.45%, 96.81% / 0.94%, 98.60% / 1.65%, 97.96% / 1.38% and 99.22 % / 1.24%. Conclusion: This method is simple, accurate, reproducible and can be used as a quality control method for panacea.