医药导报
醫藥導報
의약도보
HERALD OF MEDICINE
2015年
7期
955-958
,共4页
徐杨璐%赵胜男%刘素丽%李守拙
徐楊璐%趙勝男%劉素麗%李守拙
서양로%조성남%류소려%리수졸
黄芩%液相色谱-质谱联用法%贮存期%含量测定
黃芩%液相色譜-質譜聯用法%貯存期%含量測定
황금%액상색보-질보련용법%저존기%함량측정
Scutellaria baicalensis Georgi%Liquid chromatography-mass spectrometry ( LC-MS )%Storage%Content determination
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。
目的：採用液相色譜-質譜聯用法測定不同貯存期黃芩中黃芩苷、漢黃芩苷、黃芩素、漢黃芩素、白楊素和韆層紙素含量,攷察黃芩貯存穩定性。方法採用Agilent Zorbax XDB-C18柱(2.1 mm×150 mm,3.5μm),流動相為乙腈-0.1%甲痠水溶液,梯度洗脫,流速0.2 mL·min-1,檢測波長276 nm,採用電噴霧正離子模式電離(ESI+),6種被測成分的鑑測離子對分彆為447/271(黃芩苷)、461/285(漢黃芩苷)、271/123(黃芩素)、285/270(漢黃芩素)、255/153(白楊素)、285/270(韆層紙素)。結果黃芩苷、漢黃芩苷、黃芩素、漢黃芩素、白楊素、韆層紙素的濃度分彆在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範圍內與各自峰麵積積分值呈良好線性關繫；測得貯存前3箇月黃芩中黃芩苷、漢黃芩苷、黃芩素、漢黃芩素、白楊素、韆層紙素含量整體呈下降趨勢,0~18箇月含量變化均不明顯。結論該實驗結果可為進一步製定黃芩質量標準提供依據。
목적：채용액상색보-질보련용법측정불동저존기황금중황금감、한황금감、황금소、한황금소、백양소화천층지소함량,고찰황금저존은정성。방법채용Agilent Zorbax XDB-C18주(2.1 mm×150 mm,3.5μm),류동상위을정-0.1%갑산수용액,제도세탈,류속0.2 mL·min-1,검측파장276 nm,채용전분무정리자모식전리(ESI+),6충피측성분적감측리자대분별위447/271(황금감)、461/285(한황금감)、271/123(황금소)、285/270(한황금소)、255/153(백양소)、285/270(천층지소)。결과황금감、한황금감、황금소、한황금소、백양소、천층지소적농도분별재8.86~177.2,2.33~46.5,2.6~52.0,0.52~10.4,0.04~0.8,0.04~0.8μg·mL-1범위내여각자봉면적적분치정량호선성관계；측득저존전3개월황금중황금감、한황금감、황금소、한황금소、백양소、천층지소함량정체정하강추세,0~18개월함량변화균불명현。결론해실험결과가위진일보제정황금질량표준제공의거。
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.
