中国药师
中國藥師
중국약사
CHINA PHARMACIST
2015年
8期
1299-1301,1302
,共4页
贝母%含量测定%优化%贝母素甲%贝母素乙%高效液相色谱-蒸发光散射检测器
貝母%含量測定%優化%貝母素甲%貝母素乙%高效液相色譜-蒸髮光散射檢測器
패모%함량측정%우화%패모소갑%패모소을%고효액상색보-증발광산사검측기
Fritillaria%Content determination%Optimization%Peimine%Peiminine%HPLC-ELSD
目的::优化3种贝母中生物碱贝母素甲和贝母素乙的含量测定方法。方法:采用混合溶液回流提取,调pH,再用乙醚萃取的方法制备供试品溶液。色谱柱:Shim-pack VP-ODS (250 mm ×4.6 mm,5μm),流动相:乙腈-0.02%二乙胺溶液(75∶25),流速1.0 ml·min-1,检测器为Alltech 2000ES ELSD,漂移管温度为93℃,载气流速为2.4 L·min-1。以对照溶液质量浓度的对数值与相应峰面积的对数值计算回归方程。结果:该方法能有效提取出样品中的生物碱,贝母素甲和贝母素乙分离度良好,在一定范围内,线性关系良好,3种贝母中生物碱加样回收率在95.22%~103.51%之间。结论:该方法简便易行,通用性良好,易于执行,为其他贝母类生物碱的含量测定提供了参考。
目的::優化3種貝母中生物堿貝母素甲和貝母素乙的含量測定方法。方法:採用混閤溶液迴流提取,調pH,再用乙醚萃取的方法製備供試品溶液。色譜柱:Shim-pack VP-ODS (250 mm ×4.6 mm,5μm),流動相:乙腈-0.02%二乙胺溶液(75∶25),流速1.0 ml·min-1,檢測器為Alltech 2000ES ELSD,漂移管溫度為93℃,載氣流速為2.4 L·min-1。以對照溶液質量濃度的對數值與相應峰麵積的對數值計算迴歸方程。結果:該方法能有效提取齣樣品中的生物堿,貝母素甲和貝母素乙分離度良好,在一定範圍內,線性關繫良好,3種貝母中生物堿加樣迴收率在95.22%~103.51%之間。結論:該方法簡便易行,通用性良好,易于執行,為其他貝母類生物堿的含量測定提供瞭參攷。
목적::우화3충패모중생물감패모소갑화패모소을적함량측정방법。방법:채용혼합용액회류제취,조pH,재용을미췌취적방법제비공시품용액。색보주:Shim-pack VP-ODS (250 mm ×4.6 mm,5μm),류동상:을정-0.02%이을알용액(75∶25),류속1.0 ml·min-1,검측기위Alltech 2000ES ELSD,표이관온도위93℃,재기류속위2.4 L·min-1。이대조용액질량농도적대수치여상응봉면적적대수치계산회귀방정。결과:해방법능유효제취출양품중적생물감,패모소갑화패모소을분리도량호,재일정범위내,선성관계량호,3충패모중생물감가양회수솔재95.22%~103.51%지간。결론:해방법간편역행,통용성량호,역우집행,위기타패모류생물감적함량측정제공료삼고。
To establish an optimized determination method for the alkaloids peimine and peiminine in three varieties of Fritillaria. Methods:The samples were refluxed in a mixed solution, the pH value of the mixed solution was adjusted, and then the solution was extracted by ether to obtain the test solution. A Shim-pack VP-ODS column (4. 6 mm × 250 mm,5 μm) was used, the mobile phase consisted of acetonitrile-0. 02% diethylamine(75∶25), and the flow rate was 1. 0 ml·min-1. An Alltech 2000ES ELSD detector was used, the drift tube temperature and the flow rate of nitrogen carrier gas in the ELSD was set at 93℃ and 2. 4 L·min-1 , respectively. The regression equation was calculated between the logarithm values of the reference solution concentration and the corre-sponding peak area. Results:The method could effectively extract the alkaloids from the samples. Peimine and peiminine were well separated by the method, and showed good linearity within the respectively given ranges. The average recovery of the alkaloids in the three varieties of Fritillaria was within the range of 95. 22%-103. 51%. Conclusion: The method is simple,convenient and universal with easy operation,which provides references for the determination of alkaloids in the other varieties of Fritillaria.