[關(guān)鍵詞]
[摘要]
目的 建立UPLC-MS/MS法同時(shí)測(cè)定不同產(chǎn)地延胡索藥材中原阿片堿、鹽酸巴馬汀、脫氫紫堇堿、延胡索乙素和延胡索甲素。方法 采用Waters UPLC HSS T3 C18色譜柱(100 mm×2.1 mm,1.7 μm),以乙腈–0.1%醋酸銨為流動(dòng)相,梯度洗脫,體積流量0.3 mL/min,柱溫40℃,進(jìn)樣量5 μL。ESI正離子模式采集,采集模式:MRM(多反應(yīng)檢測(cè)),離子源溫度150℃,毛細(xì)管電壓3.0 kV,錐孔電壓50 V,脫溶劑氣流量800 L/h,脫溶劑氣溫度400℃。結(jié)果 原阿片堿、鹽酸巴馬汀、脫氫紫堇堿、延胡索乙素和延胡索甲素分別在0.20~10.12、0.25~12.58、1.02~51.20、0.85~42.64、0.39~19.44 ng線性關(guān)系良好;平均回收率分別為97.48%、100.16%、101.61%、96.05%、104.17%,RSD值分別為1.70%、2.05%、2.55%、0.74%、3.24%。不同產(chǎn)地的延胡索藥材中5種生物堿的含量有明顯差異,浙江產(chǎn)地延胡索藥材中5種生物堿的含量相對(duì)其他產(chǎn)地較高,5種生物堿中脫氫紫堇堿的含量最高。結(jié)論 UPLC-MS/MS法靈敏度高、測(cè)定速度快、準(zhǔn)確度高,可用于延胡索藥材中5種成分的快速測(cè)定。
[Key word]
[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
[中圖分類號(hào)]
R286.02
[基金項(xiàng)目]