[关键词]
[摘要]
目的 建立同时快速测定木瓜饮片中莽草酸、柠檬酸、原儿茶酸、绿原酸、咖啡酸、肉桂酸、齐墩果酸、熊果酸8种有机酸的超高速液相色谱-质谱(UFLC-MS)分析方法。方法 采用岛津LC-20A快速液相系统,AB Sciex Qtrap 5500型三重四级杆线性离子阱质谱仪,Poroshell 120色谱柱(100 mm×4.6 mm,2.7 μm);流动相为0.5%醋酸水溶液(A)-0.5%醋酸甲醇溶液(B),梯度洗脱:0~5 min,10% A;5~13 min,10%~30% A;13~15 min,30%~95% A;15~25 min,95% A;分析时间25 min;体积流量0.6 mL/min;柱温30 ℃;进样量2 μL。采用电喷雾离子源进行负离子模式检测,多反应监测模式(MRM)用于定量分析,源喷射电压为-4 500 V,离子源温度为550 ℃。结果 测定的8种成分在线性范围内均具有良好的线性关系(r≥0.999 2),平均回收率在96.14%~101.20%。不同产地的木瓜饮片中8种成分的量差异较大,其中,柠檬酸、绿原酸、莽草酸的量较高,咖啡酸的量最低。结论 建立的测定方法重复性好,且快速、灵敏度高,可为木瓜饮片的质量控制提供依据以及方法学支持。
[Key word]
[Abstract]
Objective To establish an UFLC-MS method for simultaneous determination of eight active components (shikimic acid, citric acid, protocatechuate, chlorogenic acid, caffeic acid, cinnamic acid, oleanolic acid, and ursolic acid). Methods Shimadzu LC-20A system was used, equipped with AB Sciex Qtrap 5500. The analysis was performed on a Poroshell 120 column (100 mm× 4.6 mm, 2.7 μm). The eight components were separated in 25 min with gradient mobile phase consisting of 0.5% CH3COOH-H2O (A) and 0.5% CH3COOH-CH3OH (B): 0—5 min, 10% A; 5—13 min, 10%—30% A; 13—15 min, 30%—95% A; 15—25 min, 95% A. The temperature of column was 30 ℃, and the injection volume was 2 μL. The multiple-reaction monitoring scanning (MRM) was employed for the quantification with switching electrospray ion source polarity in negative mode. The ion spray voltage was set at -4 500 V and the turbo spray temperature was maintained at 550 ℃. Results The eight components had a good linearity (r ≥ 0.999 2) within the linear ranges. The average recoveries were 96.14%—101.20%. The contents of the eight components in Chaenomelis Fructus varied from the different habitats. The contents of shikimic acid, citric acid, and chlorogenic acid were high while the content of caffeic acid was low. Conclusion The developed UFLC-MS method is simple, sensitive, and accurate and has the good repeatability in separation, which is available for the quality control of Chaenomelis Fructus.
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[基金项目]
江苏省中药资源产业化过程协同创新中心项目(ZDXM-1-3);江苏高校优势学科建设工程资助项目(ysxk-2014);江苏高校品牌专业建设工程资助项目(PPZY2015A070)