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[摘要]
目的 建立柱前皂化HPLC测定不同产地桃仁脂肪酸中亚油酸、油酸的测定方法,为有效控制和科学评价桃仁药材质量提供依据。方法 桃仁以0.5 mol/mL氢氧化钾乙醇溶液皂化提取亚油酸、油酸,利用HPLC测定桃仁中亚油酸、油酸的量。色谱柱:Waters-Symmetry-RP-C18(250 mm×4.6 mm,5 μm),流动相为乙腈-0.1%磷酸水溶液(92∶8),体积流量1.0 mg/mL,检测波长205 nm,柱温30 ℃。结果 亚油酸进样量在8.193 2~163.864 μg/mL具有良好的线性关系(r=0.999 7),平均回收率为97.3%,RSD为2.7%;油酸进样量26.4~528.0 μg/mL具有良好的线性关系(r=0.999 5),平均回收率为98.0%,RSD为2.3%。结论 本方法准确,重复性好,简便易行,适用于桃仁脂肪酸中亚油酸、油酸的同时测定。
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[Abstract]
Objective To develop a precolumn saponification HPLC method for determining linolic acid and oleic acid in Persicae Semen from different habitats and to provide the basis for controlling the herb quality quickly and accurately. Methods The linolic acid and oleic acid in Persicae Semen were saponified with 0.5 mol/mL KOH/EtOH as saponifier. HPLC method was used to determine the contents of linolic acid and oleic acid. The column was Waters-Symmetry-RP-C18 (250 mm × 4.6 mm, 5 μm), the mobile phase consisted of acetonitrile-0.1% aqueous phosphoric acid (92︰8); The flow rate was 1.0 mg/mL; The absorbance was monitored at 205 nm; The column temperature was 30 ℃. Results The calibration curves of linolic acid and oleic acid were in a good linearity over the ranges of 8.193 2—163.864 μg/mL (r = 0.999 7) and 26.4—528.0 μg/mL (r = 0.999 5), and the average recoveries of linolic acid and oleic acid were 97.3% and 98.0% with RSD values of 2.7% and 2.3%, respectively (n = 6). Conclusion This method is simple, sensitive, and accurate, which is suitable for the simultaneous determination of linolic acid and oleic acid in Persicae Semen.
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[基金项目]
国家“重大新药创制”科技重大专项(2009ZX09504-004)