[关键词]
[摘要]
目的 建立同时测定天麻饮片中天麻素、对羟基苯甲醇、香荚兰醇、对羟基苯甲醛、香荚兰醛、巴利森苷B、巴利森苷C、巴利森苷A 8种成分的高效液相色谱-质谱(HPLC-MS)分析方法。方法 采用Agilent 1220高效液相系统,Hypersil C18色谱柱(250 mm×4.6 mm,5 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:0~10 min,98% A;10~60 min,98%~60% A;60~75 min,60% A;分析时间75 min;体积流量0.8 mL/min;柱温30 ℃;进样量20 μL。采用电喷雾离子源进行负离子模式监测,多反应监测模式用于定量分析,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94.51%~102.70%,RSD < 3.50%。在不同产地的天麻饮片中,8种成分的量差异较大。其中,3种巴利森苷类成分的量较高,香荚兰醇和香荚兰醛的量均较低。结论 建立的测定方法分离效果及重复性好,且快速、简便,可作为天麻饮片的质量控制方法。
[Key word]
[Abstract]
Objective To establish an HPLC method for the simultaneous determination of eight active components (gastrodin, 4-hydroxybenzyl alcohol, vanillyl alcohol, vanillin, p-hydroxybenzaldehyde, parishin B, parishin C, and parishin A). Methods The analysis was performed on an Agilent 1220 system with a Hypersil C18 column (250 mm × 4.6 mm, 5 μm). The eight components were separated in 75 min with gradient mobile phase consisting of 0.5% CH3COOH-H2O (A) and 0.5% CH3COOH-CH3OH (B): 0—10 min, 98% A; 10—60 min, 98%—60% A; 60—75 min, 60% A. The temperature of column was 30 ℃, and the injection volume was 20 μL. The multiple-reaction monitoring (MRM) scanning was employed for the quantification with switching electrospray ion source polarity in negative mode. The ion spray voltage was set at -4500 V and the turbo spray temperature was maintained at 550 ℃. Results The eight components had the good linearity (r ≥ 0.999 2) within the linear ranges. The average recovery rate was 94.51%—102.70% with RSD < 3.50%. The contents of the eight components of Gastrodiae Rhizoma varied according to the different habits. The contents of parishins A, B, and C were high while the contents of vanillyl alcohol and vanillin were low. Conclusion The developed HPLC-MS method is simple, sensitive, and accurate, and has the good repeatability in separation, which is available for the quality control of Gastrodiae Rhizoma.
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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