摘要
目的：通过高效液相色谱-质谱串联（ HPLC-MS/MS）法鉴定阴地蕨中山奈酚成分，并建立HPLC法同时测定阴地蕨中山奈酚和槲皮素含量。方法采用 Agilent 1200 LC高效液相色谱仪及 API3200 QTRAP MS/MS质谱仪， Ecilipse XDB-C18（15 mm×4.6 mm，5μm）色谱柱，甲醇-0.1％甲酸溶液（85：15）为流动相，鉴定阴地蕨中山奈酚及槲皮素；用Agilent 1260 LC高效液相色谱仪，Eclipse plus C18色谱柱（100 mm×4.6 mm，5μm），甲醇-0.4％磷酸溶液（45：55）为流动相，流速0.8 mL·min－1，检测波长360 nm，测定阴地蕨中的山奈酚及槲皮素含量。结果出现m/z 287.1[M＋H]＋及m/z 301.0[ M＋H]＋峰为质谱的特征峰，分别与山奈酚及槲皮素对照品具有高相似度，证明样品中含有山奈酚和槲皮素；山奈酚和槲皮素的线性范围均为2.500~25.000μg·mL－1，r分别为0.9999和0.9998；精密度实验RSD分别为0.98％和0.79％（ n＝5）；加样回收率RSD分别为1.89％，2.70％（ n＝5）。结论阴地蕨中含有丰富的山奈酚及槲皮素，HPLC法适于同时测定阴地蕨中的山奈酚及槲皮素含量，方法简便可行，重复性好，精密度高，结果可靠。
Objective To establish a method for simultaneous determination of kaempferol and quercetin in Botrychium ternatum （ a kind of Ethnic Chinese herbal medicine） by HPLC and HPLC-MS/MS. Methods Agilent 1200 HPLC, API3200 QTRAP MS/MS, Ecilipse XDB-C18 column （15 mm×4.6 mm, 5μm） and the mobile phase consisting of methanol-0.1%formic-water （85：15） were applied to identify kaempferol and quercetin in Botrychium ternatum;Agilent 1260 HPLC and Eclipse plus C18（100 mm×4.6 mm, 5 μm） column were used for determination of the two.The mobile phase was a mixture of methanol and 0.4% phosphoric acid solution （45：55） with a flow rate of 0.8 mL·min-1 and the detection wavelength was 360 nm. Results In mass spectrogram of Botrychium ternatum, characteristic peaks of m/z 287. 1 [ M＋H]＋ and m/z 301.0 [ M＋H]＋ were consistent with those of standard sample of kaempferol and quercetin, which confirmed their existence in Botrychium ternatum.The two flavonoids both had a good linearity in the range of 2.500–25.00μg·mL-1（r = 0.999 9 and 0.999 8, respectively）.RSD of precision and reproducibility of kaempferol and quercetin were 0.98%,1.89% and 0.79%,2.70%, respectively. Conclusion The method is simple, accurate with high sensitivity and suitable for the determination of kaempferol and quercetin in Botrychium ternatum.
出处
《医药导报》
CAS
2015年第10期1360-1363,共4页
Herald of Medicine
基金
国家社会科学基金资助项目(12XMZ033)
