医药导报
醫藥導報
의약도보
Herald of Medicine
2015年
10期
1360-1363
,共4页
阴地蕨%山奈酚%槲皮素%高效液相色谱-质谱串联法
陰地蕨%山奈酚%槲皮素%高效液相色譜-質譜串聯法
음지궐%산내분%곡피소%고효액상색보-질보천련법
Botrychium ternatum%Kaempferol%Quercetin%HPLC-MS/MS
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。
目的：通過高效液相色譜-質譜串聯( HPLC-MS/MS)法鑒定陰地蕨中山奈酚成分，併建立HPLC法同時測定陰地蕨中山奈酚和槲皮素含量。方法採用 Agilent 1200 LC高效液相色譜儀及 API3200 QTRAP MS/MS質譜儀， Ecilipse XDB-C18(15 mm×4.6 mm，5μm)色譜柱，甲醇-0.1％甲痠溶液(85??15)為流動相，鑒定陰地蕨中山奈酚及槲皮素；用Agilent 1260 LC高效液相色譜儀，Eclipse plus C18色譜柱(100 mm×4.6 mm，5μm)，甲醇-0.4％燐痠溶液(45??55)為流動相，流速0.8 mL??min－1，檢測波長360 nm，測定陰地蕨中的山奈酚及槲皮素含量。結果齣現m/z 287.1[M＋H]＋及m/z 301.0[ M＋H]＋峰為質譜的特徵峰，分彆與山奈酚及槲皮素對照品具有高相似度，證明樣品中含有山奈酚和槲皮素；山奈酚和槲皮素的線性範圍均為2.500~25.000μg??mL－1，r分彆為0.9999和0.9998；精密度實驗RSD分彆為0.98％和0.79％( n＝5)；加樣迴收率RSD分彆為1.89％，2.70％( n＝5)。結論陰地蕨中含有豐富的山奈酚及槲皮素，HPLC法適于同時測定陰地蕨中的山奈酚及槲皮素含量，方法簡便可行，重複性好，精密度高，結果可靠。
목적：통과고효액상색보-질보천련( HPLC-MS/MS)법감정음지궐중산내분성분，병건립HPLC법동시측정음지궐중산내분화곡피소함량。방법채용 Agilent 1200 LC고효액상색보의급 API3200 QTRAP MS/MS질보의， Ecilipse XDB-C18(15 mm×4.6 mm，5μm)색보주，갑순-0.1％갑산용액(85??15)위류동상，감정음지궐중산내분급곡피소；용Agilent 1260 LC고효액상색보의，Eclipse plus C18색보주(100 mm×4.6 mm，5μm)，갑순-0.4％린산용액(45??55)위류동상，류속0.8 mL??min－1，검측파장360 nm，측정음지궐중적산내분급곡피소함량。결과출현m/z 287.1[M＋H]＋급m/z 301.0[ M＋H]＋봉위질보적특정봉，분별여산내분급곡피소대조품구유고상사도，증명양품중함유산내분화곡피소；산내분화곡피소적선성범위균위2.500~25.000μg??mL－1，r분별위0.9999화0.9998；정밀도실험RSD분별위0.98％화0.79％( n＝5)；가양회수솔RSD분별위1.89％，2.70％( n＝5)。결론음지궐중함유봉부적산내분급곡피소，HPLC법괄우동시측정음지궐중적산내분급곡피소함량，방법간편가행，중복성호，정밀도고，결과가고。
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.
