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作 者:许可[1] 朱冬青[1] 蔡进章[2] 赖敏敏 王贤亲[3] 林崇良[1]
机构地区:[1]温州医科大学附属第一医院药学部,325000 [2]温州医科大学附属第二医院药学部 [3]温州医科大学药学院分析测试中心
出 处:《中国医药》2014年第10期1552-1556,共5页China Medicine
摘 要:目的 建立药根碱、巴马汀和小檗碱的含量测定的高效液相色谱法,并测定不同产地功劳木中药根碱、巴马汀和小檗碱含量.方法 样品用盐酸-甲醇(体积比1∶100)混昆合溶液超声提取,采用高效液相色谱法,色谱柱为Agilent ZORBAX SB-C18(150mm×2.1 mm,5μm),以甲醇-0.1%甲酸为流动相,流速为0.4 ml/min,柱温为40℃,检测波长为345 nm.配制一系列质量浓度(X)梯度的药根碱溶液(1.00、5.00、25.00、50.00、75.00、100.00 mg/L)、小檗碱溶液(l.00、2.50、5.00、25.00、75.00、100.00 mg/L)和巴马汀溶液(0.11、0.55、2.20、11.00、22.00、44.00 mg/L).分别取5μl注入高效液相色谱仪并记录药根碱、小檗碱和巴马汀的峰面积(Y).以浓度(X)为横坐标,色谱峰面积(y)为纵坐标绘制标准曲线,计算回归方程.取庆元百山祖、五凤垟麻宅村、泽雅源口、瓯海泽雅4个不同产地的功劳木药材,测定药根碱、小檗碱、巴马汀峰面积,每个样品测定3次.结果 上述色谱条件下,药根碱、巴马汀和小檗碱可以较好地分离,线性范围分别是0.005 00 ~0.500 00μg(r =0.999 9)、0.00500~ 0.750 00μg(r =0.999 8)、0.000 55 ~0.22000μg(r =0.999 5),平均回收率分别为98.47%[相对标准偏差(RSD)=2.84%]、98.58% (RSD=3.34%)、99.58%(RSD=3.76%).不同产地功劳木3种生物碱总量有差异,庆元百山祖阔叶功劳木、五凤垟麻宅村功劳木、泽雅源口阔叶功劳木、瓯海泽雅阔叶功劳木的药根碱、巴马汀和小檗碱的总含量分别为7.42、16.18、13.20、20.36 mg/g,最高相差3倍;药根碱含量分别为3.91、8.06、3.78、7.91 mg/g,小檗碱含量分别为1.42、7.64、8.61、10.55 mg/g,巴马汀含量分别为2.10、0.48、0.80、1.90 mg/g.3种生物碱含量高低与原植物品种、温度、日照强度及产地有关.结论 高效液相色谱法测定药根碱、巴马汀和小檗碱的含量简便、快速、重现性好,适用�Objective To establish a liquid chromatography method for determination of Jatrorrhizine,Palmatine and Berberine in Mahonia from different areas by high pressure liquid chromatography.Methods The sample was treated by ultrasonic extraction with HCl-MeOH (1∶ 100,by volume).The analytical column was the Agilent ZORBAX SB-C18Column (150mm × 2.1mm,5μm).The mobile phase consisted of Methanol-0.1% Formic acid,the flow rate was 0.4 ml/min,the column temperature was 40 ℃ and the detection wavelength was 345 nm.Results The calibrated linear curves of jatrorrhizine,palmatine and berberine concentrations were within the range of 0.005 00-0.500 00,0.005 00-0.750 00 and 0.000 55-0.220 00μg; the correlation coefficients (r) were 0.999 9,0.999 8 and 0.999 5,respectively.The recovery rates were 98.47% (RSD =2.84%),98.58% (RSD =3.34%) and 99.58% (RSD =3.76%).There was a significant difference between the total amounts of alkaloids in Mahonia from different areas.They were 7.42,13.20,16.18 and 20.36 mg/g respectively.The maximum was 3 times higher than that of the minimum.The content of Jatrorrhizine was 3.91,8.06,3.78,7.91 mg/g,respectively.The Berberine was 1.42,7.64,8.61 and 10.55 mg/g; the Palmatine was 2.10,0.48,0.80 and 1.90 mg/g.The contents of the 3 alkaloids were related to the original plant variety,temperature,sunshine intensity and producing area.Conclusions The method is simple and fast.It can be used for simultaneous determination of Jatrorrhizine,Palmatine,Berberine in Mahonia.
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