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[摘要]
目的 建立UPLC-MS/MS法同时测定不同产地延胡索药材中原阿片碱、盐酸巴马汀、脱氢紫堇碱、延胡索乙素和延胡索甲素。方法 采用Waters UPLC HSS T3 C18色谱柱(100 mm×2.1 mm,1.7 μm),以乙腈–0.1%醋酸铵为流动相,梯度洗脱,体积流量0.3 mL/min,柱温40℃,进样量5 μL。ESI正离子模式采集,采集模式:MRM(多反应检测),离子源温度150℃,毛细管电压3.0 kV,锥孔电压50 V,脱溶剂气流量800 L/h,脱溶剂气温度400℃。结果 原阿片碱、盐酸巴马汀、脱氢紫堇碱、延胡索乙素和延胡索甲素分别在0.20~10.12、0.25~12.58、1.02~51.20、0.85~42.64、0.39~19.44 ng线性关系良好;平均回收率分别为97.48%、100.16%、101.61%、96.05%、104.17%,RSD值分别为1.70%、2.05%、2.55%、0.74%、3.24%。不同产地的延胡索药材中5种生物碱的含量有明显差异,浙江产地延胡索药材中5种生物碱的含量相对其他产地较高,5种生物碱中脱氢紫堇碱的含量最高。结论 UPLC-MS/MS法灵敏度高、测定速度快、准确度高,可用于延胡索药材中5种成分的快速测定。
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[Abstract]
Objective To establish a method for the simultaneous determination of protopine, palmatinechloride, dehydrocorydaline, tetrahydropalmatine, and corydaline in Corydalis Rhizoma by UPLC-MS/MS. Methods Waters HSS T3 C18 column (100 mm×2.1 mm, 1.7 μm) was used with mobile phase consisted of acetonitrile-0.1% ammonium acetate by gradient elution. The column temperature was 40℃ and the volume of injection was 5 μL with flow rate of 0.3 mL/min. Multiple-reaction monitoring scanning was used for quantification with electrospray positive ions model. The ion source temperature was 150℃, the capillary voltage was 3.0 kV, the cone voltage was 50 V, the desolvation gas flow rate was 800 L/h, and the desolvation gas temperature was 400℃. Results The linear ranges of protopine, palmatinechloride, dehydrocorydaline, tetrahydropalmatine, and corydaline were 0.20-10.12 ng, 0.25-12.58 ng, 1.02-51.20 ng, 0.85-42.64 ng, and 0.39-19.44 ng, respectively. The average recoveries were 97.48%, 100.16%, 101.61%, 96.05%, and 104.17% with RSD of 1.70%, 2.05%, 2.55%, 0.74%, and 3.24%, respectively. The contents of five alkaloids in Corydalis yanhusuo from different origins were obviously different. The contents of five alkaloids in Corydalis Rhizoma from Zhejiang Province origin were higher than those of other origins, and the content of dehydrocordine was the highest among the five alkaloids. Conclusion The established method is easy, rapid, and accurate which can be used for the content determination of five alkaloids in Corydalis Rhizoma
[中图分类号]
R286.02
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