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作 者:叶凡[1] 周邦华[1] 王胜[1] 李艳[1] 范刚[1] 赖先荣[1]
出 处:《时珍国医国药》2016年第2期286-289,共4页Lishizhen Medicine and Materia Medica Research
基 金:国家自然科学基金(No.81173360;No.81303310;No.81473427;No.81560806);四川省科技厅科技支撑计划(No.2011SZ0298);四川省教育厅重点项目(No.10ZA092);四川省高校科研创新团队建设计划项目(No.11TD004)
摘 要:目的建立藏药小檗膏提取物中3种生物碱(盐酸药根碱、盐酸巴马汀、盐酸小檗碱)的含量测定方法。方法采用HPLC法,色谱柱为Wondasil C18-WR柱(4.6 mm×250 mm,5μm);流动相A为0.3%磷酸水溶液,流动相B为乙腈,梯度洗脱(0~5 min,23%B;5~27 min,23%→26%B;27~32 min,26%→35%B;32~35 min,35%→23%B;35~45 min,23%B),流速为1.0 ml·min-1,柱温为30℃,检测波长为345 nm。结果 3种生物碱分别在4.3886~87.7716(r=0.9997)、3.6649~73.2982(r=0.9998)、29.5994~591.9876(r=0.9999)μg·ml-1范围内线性关系良好(n=8);平均加样回收率(n=9)分别为97.97%(RSD=1.02%)、100.70%(RSD=1.42%)、98.51%(RSD=0.86%)。测定5个批次小檗膏提取物,以干燥品计,3种生物碱平均含量分别为12.9553,5.4508,46.1840 mg·g-1。结论建立的3种生物碱含量方法简便准确,重复性好,可作为藏药小檗膏提取物的质量控制方法。Objective To establish a content determination method of three alkaloids( Jatrorrhizine Hydrochloride,Palmatine Hydrochloride and Berberine Hydrochloride) in Tibetan Medicine Berberis Cortex Cream( TMBCC). Methods The content of three alkaloids was determined by high performance liquid chromatography( HPLC). The chromatographic column was Wondasil C18- WR( 4. 6 mm × 250 mm,5 μm). The mobile phases were 0. 3% phosphoric acid water solution as mobile phase A and acetonitrile as mobile phase B with gradient elution( 0- 5 min,23 % B; 5- 27 min,23 % →26 % B; 27- 32 min,26 % →35% B; 32- 35 min,35 % →23 % B; 35- 45 min,23 % B) at rate 1. 0 ml·min- 1. The column temperature was set as 30 ℃.The detection wavelength was set at 345 nm. Results The linear ranges( n = 8) for three alkaloids were 4. 3886 ~ 87. 7716 μg·m L- 1( r = 0. 9997),3. 6649 ~ 73. 2982 μg·m L- 1( r = 0. 9998),29. 5994 ~ 591. 9876 μg·m L- 1( r = 0. 9999). The average recoveries( n = 9) for three alkaloids were 97. 97%( RSD = 1. 02%),100. 70%( RSD = 1. 42%),98. 51%( RSD = 0. 86%),while the five samples average contents were 12. 9553,5. 4508,46. 1840 mg·g- 1,respectively. Conclusion The method is simple,accurate and has a good stability,can be used for the content determination in processed products of TMBCC.
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