建立了高效液相色谱快速定量测定中药千层塔提取物中石杉碱甲含量的分析方法。千层塔提取物经甲醇/水/甲酸(10/90/0.2,v/v/v)提取并定容后,过滤膜后直接分析。色谱分离选用XCharge C18色谱柱(150mm×4.6mm,5μm),以水(含0.1%三氟乙酸)和乙腈(含0.09%三氟乙酸)为流动相进行梯度洗脱,流速为2mL/min,于310nm波长下检测,可在10min内完成石杉碱甲的快速分离分析。结果表明,石杉碱甲在2.12-106mg/L范围内线性关系良好(相关系数为0.9999);平均加标回收率为102.34%,相对标准偏差(RSD)为0.46%;日内及日间精度均小于2%,满足下量要求。该方法简便、快速、结果可靠、可现性好,可作为千层塔提取质量评价的依据。
A high performance liquid chromatographic (HPLC) method was established to determine the Huperzine A in the extract of Huperzia serrata. After extracted by methanol/ water/formic acid ( 10/90/0.2, v/v/v), the sample was filtered for HPLC analysis. The separa- tion was performed on an XCharge C18 column ( 150 mm ×4.6 mm, 5 μm) by gradient elution with water ( containing 0. 1% (v/v) trifluoroacetic acid ) and acetonitrile ( containing 0.09% (v/v) trifluoroacetic acid) as the mobile phases. Rapid separation was achieved within 10 rain at a flow rate of 2 mL/min with ultraviolet absorption detection at a wavelength of 310 nm. Under the optimized conditions, good linearity was obtained in the range of 2. 12 - 106 mg/L with the correlation coefficient (R2 ) of about 0. 999 9. The average recovery was 102.34% with the relative standard deviation (RSD) of 0.46%. The intraday and interday precisions were all below 2%. The results demonstrate that this method is simple, rapid and accurate with good reproducibility, and can be used to evaluate the quality of Huperzia serrata.