干姜药材不同提取液HPLC-MSD指纹图谱研究

A Study on HPLC-MSD Chromatographic Fingerprints of Different Extracts of Dried Ginger

目的对干姜药材不同提取液高效液相-质谱检测器(HPLC-MSD)总离子流色谱指纹图谱的方法学进行评价。方法确定试验条件并进行方法学考察,色谱条件:Agilent Zorbax SB C18色谱柱(4.6μm×250.0μm,5.0μm);流动相A相为乙腈,B相为水,梯度洗脱;流速1.0 ml/min,柱后分流;柱温25℃;进样量10μl。质谱条件:大气压电离-电喷雾电离(API-ESI)离子源,正离子检测模式,质荷比200～1200,干燥气(N2)流速10 L/min,雾化气压力0.58 mmHg(30 psig),干燥气温度350℃,裂解电压70 V,毛细管电压3500 V。结果干姜药材HPLC-MSD总离子流色谱指纹图谱具有较好的稳定性、精密度和重复性,相对保留时间和相对峰面积的相对标准偏差均<3.0%。干姜药材甲醇提取液HPLC-MSD总离子流指纹图谱中色谱峰分离较好,确定了20个特征色谱峰;干姜药材水煎液中色谱峰明显少于甲醇提取液,色谱图中仅检测到4～8号色谱峰。结论本研究可为干姜药材指纹图谱的系统研究提供有益借鉴,同时有助于干姜药材的质量控制和评价。

Objective To establish evaluation mechanisms of different extracts of dried ginger by HPLC-MSD total ionic chromatographic fingerprints.Methods The conditions of experiment were confirmed and the validation of the method was also evaluated.The chromatography conditions were with Agilent zorbax SB Cl8 column(4.6 μm×250 μm,5.0 μm);mobile phase was A: ACN,B: H2O,gradient elution;flow speed was 1.0 ml/min,distributary after column,temperature of column was 25℃,injection volume 10 μl.The mass spectrum conditions were with atmosphere pressure ionization-electrospray(API-ESI),positive scan mode with mass change ratio was in a range from 200 to 1200,drying gas(N2) flow was 10 L/min,nebulizer pressure was 0.58 mmHg(30 psig),drying gas temperature was 350 ℃,fragment voltage was 70 V,and capillary voltage was 3500 V.Results HPLC-MSD total ionic chromatographic fingerprints of dried ginger showed better stability,precision and reproducibility,RSD of relative retention of times and peak areas were fewer than 3.0%.Methanol extract for HPLC-MSD total ionic chromatographic fingerprints was better separated,and 20 characteristic peaks were confirmed.Water extract had fewer peaks than methanol extract,and only no.4 to 8 peaks were found in chromatogram.Conclusion The study is helpful in the system research of chromatographic fingerprint of dried ginger,and evaluation of the quality of dried ginger.