液质联用法测定不同贮存期黄芩中6种黄酮类化合物含量  

Determination of Six Kinds of Flavonoids in Scutellaria baicalensis Georgi with Different Storage Time by LC-MS

作　　者：徐杨璐 赵胜男[1] 刘素丽[1] 李守拙[1] 

机构地区：[1]承德医学院河北省中药研究与开发重点实验室,承德067000

出　　处：《医药导报》2015年第7期955-958,共4页Herald of Medicine

基　　金：国家科技支撑计划(2011BAI07B04)

摘　　要：目的 采用液相色谱-质谱联用法测定不同贮存期黄芩中黄芩苷、汉黄芩苷、黄芩素、汉黄芩素、白杨素和千层纸素含量,考察黄芩贮存稳定性。方法 采用Agilent Zorbax XDB-C18柱（2.1 mm×150 mm,3.5μm）,流动相为乙腈-0.1%甲酸水溶液,梯度洗脱,流速0.2 m L·min-1,检测波长276 nm,采用电喷雾正离子模式电离（ESI＋）,6种被测成分的监测离子对分别为447/271（黄芩苷）、461/285（汉黄芩苷）、271/123（黄芩素）、285/270（汉黄芩素）、255/153（白杨素）、285/270（千层纸素）。结果 黄芩苷、汉黄芩苷、黄芩素、汉黄芩素、白杨素、千层纸素的浓度分别在886~1 772,23.3~465,26~520,5.2~104,0.4~8,0.4~8μg范围内与各自峰面积积分值呈良好线性关系;测得贮存前3个月黄芩中黄芩苷、汉黄芩苷、黄芩素、汉黄芩素、白杨素、千层纸素含量整体呈下降趋势,0~18个月含量变化均不明显。结论该实验结果可为进一步制定黄芩质量标准提供依据。Objective To quantify the contents of baicalin, wogonoside, baicalein, wogonin, chrysim and oroxylinA in the Scutellaria baicalensis Georgi with different storage time by liquid chromatography-mass spectrometry（ LC-MS） and determine the stability of Scutellaria baicalensis Georgi. Methods The LC system consisted of an Agilent Zorbax XDB-C18 column （2. 1 mm×150 mm,3. 5 μm） with acetonitrile and water （0. 1% formic acid） in linear gradient condition. The flow rate was 0. 2 mL·min-1 and the wavelength of detection was 276 nm. The mass spectrometer was operated under the positive ion mode with the ESI source. The precursor-to-product ion pair was 447/271 for baicalin,461/285 for wogonoside,271/123 for baicalein, 285/270 for wogonin, 255/153 for chrysim and 285/270 for oroxylinA, respectively. Results The contents of baicalin, wogonoside, baicalein, wogonin, chrysim and oroxylin A had a linear relationship with their peak areas within the ranges of 8. 86-177. 2, 2. 33-46. 5, 2. 6-52. 0, 0. 52-10. 4, 0. 04-0. 8 and 0. 04-0. 8 μg · mL-1 , respectively. The contents of baicalin, wogonoside, baicalein, wogonin, chrysim, and oroxylin A were overall decreased over the first 3 months of storage,but remained relatively stable between 0 and 18 months. Conclusion The results provides basis for the establishment of quality standard.

关 键 词：黄芩 液相色谱-质谱联用法 贮存期 含量测定 

分 类 号：R286[医药卫生—中药学] R927.1[医药卫生—中医学]