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作 者:田菁[1] 范欣戎[2] 李晓东[2] 孙会敏[2]
机构地区:[1]中国药学杂志编辑部,北京100022 [2]中国药品生物制品检定所,北京100050
出 处:《药物分析杂志》2010年第5期810-813,共4页Chinese Journal of Pharmaceutical Analysis
摘 要:目的:建立苦豆草药材中多个生物碱同时定性定量分析的高效液相色谱法。方法:采用DiamonsilTM C18柱(5μm,250mm×4.6mm),以0.05mol.L-1磷酸二氢钠水溶液-乙腈-甲醇-高氯酸钠(940mL:50mL:10mL:25g;pH4.5)为流动相,流速1mL.min-1,检测波长210nm,柱温40℃(0~39min)→50℃(40~49min)→40℃(50~55min)。结果:本方法在55min内定性分析了宁夏市售苦豆草中9个生物碱,并对其中6个进行了定量测定。苦参碱、槐定碱、槐果碱、苦豆碱、氧化槐果碱、氧化苦参碱的浓度均在0.002~2.00mg.mL-1范围内与峰面积呈良好线性关系,平均回收率(n=3)分别为97.4%~98.3%(RSD≤1.3%),97.5%~98.3%(RSD≤1.2%),96.8%~98.0%(RSD≤1.2%),97.1%~98.0%(RSD≤1.0%),97.9%~98.3%(RSD≤1.1%),97.1%~98.7%(RSD≤0.8%)。结论:本法灵敏、准确,专属性好,适用于苦豆草药材中生物碱成分的定性鉴别和定量分析。Objective:To establish an HPLC method for the simultaneous qualitative and quantitative determination of multiple alkaloids in the whole herbs of Sophora alopecuroides.Methods:The method was conducted on a DiamonsilTM C18 column(5 μm,250 mm×4.6 mm)with 0.05 mol·L-1 sodium dihydrogen phosphate-acetonitrile-methyl alcohol-sodium perchlorate(940 mL:50 mL:10 mL:25 g;pH 4.5)as mobile phase,flow rate of 1 mL· min-1,UV detection at 210 nm and column temperature at 40 ℃(0-39 min)→50 ℃(40-49 min)→40 ℃(50-55 min).Results:Nine alkaloids in S.alopecuroides from Ningxia herbs market were identified and six of them were simultaneously determinated by the developed method in 55 min.Matrine,sophoridine,sophocarpine,aloperine,oxysophocarpine and oxymatrine all showed good linearity in the range of 0.002-2.00 mg·mL-1;The average recoveries(n=3)were 97.4%-98.3%(RSD≤1.3%),97.5%-98.3%(RSD≤1.2%),96.8%-98.0%(RSD≤1.2%),97.1%-98.0%(RSD≤1.0%),97.9%-98.3%(RSD≤1.1%),and 97.1%-98.7%(RSD≤0.8%).Conclusion:The developed method is sensitive,accurate and specific for the identification and determination of the alkaloids in the whole herbs of S.alopecuroides.
分 类 号:R917[医药卫生—药物分析学]
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