[关键词]
[摘要]
目的 建立超高效液相色谱串联质谱(UPLC-MS/MS)法测定不同产地多穗金粟兰中绿原酸、异嗪皮啶-7-O-β-D-葡萄糖苷、异嗪皮啶、4-O-β-D-吡喃糖迷迭香酸和迷迭香酸。方法 采用Waters UPLC HSS T3 C18色谱柱(100 mm×2.1 mm,1.8μm),以乙腈-0.1%甲酸为流动相,梯度洗脱,体积流量0.3 mL/min,柱温40 ℃,进样量2 μL。质谱采用电喷雾负离子模式采集,采集方式:多反应检测和多通道分段采集。结果 绿原酸、异嗪皮啶-7-O-β-D-葡萄糖苷、异嗪皮定、4-O-β-D-吡喃糖迷迭香酸和迷迭香酸分别在0.48~15.36、0.20~6.50、0.24~7.84、0.38~12.26、0.92~29.44μg/mL线性关系良好;平均回收率分别为95.19%、93.77%、92.50%、99.51%、96.96%。10批不同产地多穗金粟兰中5种成分含量差异较大。结论 方法灵敏度高、准确度高、分析速度快,可为提高多穗金粟兰药材质量标准提供参考。
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[Abstract]
Objective To develop a UPLC-MS/MS method for the quantification of chlorogenic acid, isofraxidin-7-O-β-D-glucoside, isofraxidin, 4-O-β-D-glucopyranosyl-rosmarinic acid, and rosmarinic acid in Chloranthus multistachys from different origins. Methods Waters HSS T3 C18 column (100 mm × 2.1 mm, 1.8 µm) was used, with acetonitrile - 0.1% formic acid as the mobile phase, employing gradient elution at a flow rate of 0.3 mL/min, column temperature of 40 °C, and an injection volume of 2 μL. Mass spectrometry was performed in negative ESI mode, with data acquisition methods including MRM and segmented multi-channel collection. Results The calibration curves were linear in the ranges of 0.48 — 15.36, 0.20 — 6.50, 0.24 — 7.84, 0.38 — 12.26, and 0.92 — 29.44 µg/mL for chlorogenic acid, isofraxidin-7-O-β-D-glucoside, isofraxidin, 4-O-β-D-glucopyranosyl-rosmarinic acid, and rosmarinic acid, and their average recoveries were 95.19%, 93.77%, 92.50%, 99.51% and 96.96%, respectively. The content of five constituents was obviously different in C. multistachys from different origins. Conclusion The method is high sensitive, accurate, and rapidly, which can provide the reference for the quality standard of C. multistachys.
[中图分类号]
R286.02
[基金项目]