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 mL·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8.86~177.2,2.33~46.5,2.6~52.0,0.52~10.4,0.04~0.8,0.04~0.8μg·mL-1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.
展开▼
