首页|气相色谱内标法测定小半夏汤中几种有机酸

气相色谱内标法测定小半夏汤中几种有机酸

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目的 建立毛细管柱GC法同时测定小半夏汤(半夏、生姜)中的琥珀酸、苹果酸、柠檬酸、亚油酸的方法.方法 使小半夏汤中的有机酸类成分甲酯化,毛细管柱GC法测定其含量.采用HP-5石英毛细管柱(30 m×0.53 mm×2.65μm);检测器氢火焰离子化检测器柱温程序升温,100℃保持3min,然后以5℃/min升温至220℃,保持5min,最后以10℃/min升温至280℃,保持5min;进样口温度250℃;检测器温度290℃;载气氮气;体积流量1.0 mL/min.水杨酸甲酯为内标,内标法定量.结果 小半夏汤中的琥珀酸、苹果酸、柠檬酸和亚油酸的加样回收率分别为100.16%( RSD为1.17%),99.93% (RSD=1.69%),100.63%(RSD为1.51%),99.91%(RSD为1.18%);方法精密度、重复性良好,RSD均小于2.0%.结论 本法操作简便,结果可靠,重现性好,检测快速,定量准确,可作为测定小半夏汤中有机酸的方法.
Determination of organic acids in Xiaobanxia Decoction
AIM To establish a capillary column GC method for determining organic acids ( succinic acid, malic acid, citric acid, and linoleic acid ) in Xiaobanxia Decoction ( Pinelliae Rhizoma, Zingiberis Rhizoma re-cens ).METHODS Methyesterification of four organic acids was carried out on sulfuric acid-methanol solution.The separation was performed on an HP-5 quartz capillary column ( 30 m × 0.53 mm × 2.65 μm ) with FID.The initial temperature of column was kept at 100 ℃ for 3 min, then raised to 220 × for 5 min at the rate of 5 ℃/min, and then raised to 280℃ for 5 min at the rate of 10 ℃/min.Injector temperature was 250 ℃.Detector temperature was 290 ℃.Carrier gas was nitrogen.The flow rate was 1.0 ml/min.The salicylic acid was used as internal standard.RESULTS The linear ranges of succinic acid, malic acid, citric acid and linoleic acid were 0.020 0 -0.260 0mg/mL( r = 0.999 9 ), 0.140 0-1.820 1 mg/mL ( r = 0.999 8 ), 0.200 1 -2.601 7 mg/mL ( r = 0.999 8 ) and 0.006 1 - 0.079 7 mg/mL ( r = 0.999 9 ), respectively.The average recoveries were 100.16%, 99.93%, 100.63% and 99.91% with corresponding RSDs of 1.17%, 1.69%, 1.51% and 1.18%, respectively.The RSDs of precision and accuracy of the assay were not more than 2.0% ( n = 6 ).CONCLUSION The method is rapid, accurate, reliable and can be used to determine the organic acids in Xiaobanxia Decoction.

GCXiaobanxia Decoctionorganic aciddetermination

张科卫、吴皓、崔小兵

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南京中医药大学,江苏省中药炮制重点实验室,江苏南京210029

气相色谱 小半夏汤 有机酸 定量测定

江苏省中医药管理局科技项目

LZ09027

2011

中成药
国家食品药品监督管理局,信息中心中成药信息站,上海中药行业协会

中成药

CSTPCDCSCD北大核心
影响因子:1.217
ISSN:1001-1528
年,卷(期):2011.33(8)
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