UPLC法同时测定清喉利咽颗粒中5种成分的含量

Contents Determination of Five Components in Qinghou Liyan Granule by UPLC

目的：建立同时测定清喉利咽颗粒中没食子酸、柚皮苷、橙皮苷、新橙皮苷和黄芩苷含量的方法。方法：采用超高效液相色谱法。色谱柱为ACQUITY UPLC BEH C_（18）,流动相为乙腈-0.1%磷酸（梯度洗脱）,流速为0.40 ml/min,检测波长为280 nm,柱温为30℃,进样量为1μl。结果：没食子酸、柚皮苷、橙皮苷、新橙皮苷和黄芩苷检测进样量线性范围分别为0.048-0.480μg（r=0.999 3）、0.012-0.120μg（r=0.999 9）、0.016-0.160μg（r=0.999 8）、0.022-0.220μg（r=0.999 9）、0.072-0.720μg（r=0.999 2）;定量限分别2.4、1.6、1.8、1.8、1.6 ng,检测限分别为7.5、5.0、5.6、5.6、5.0 ng;精密度、稳定性、重复性试验的RSD〈3.0%;加样回收率分别为96.64%-102.02%（RSD=2.00%,n=6）、95.86%-102.56%（RSD=2.86%,n=6）、97.24%-102.54%（RSD=2.10%,n=6）、97.44%-102.60%（RSD=2.40%,n=6）、96.91%-103.13%（RSD=2.62%,n=6）。结论：该方法快速、准确,可用于同时测定清喉利咽颗粒中没食子酸、柚皮苷、橙皮苷、新橙皮苷和黄芩苷的含量。

OBJECTIVE：To establish a method for the contents determination of gallic acid,naringin,hesperidin,neohesperidin and baicalin in Qinghou liyan granule. METHODS：UPLC was performed on the column of ACQUITY UPLC BEH C_（18） with mobile phase of acetonitrile- 0.1% phosphoric acid（gradient elution）at a flow rate of 0.40 ml/min,detection wavelength was 280 nm,column temperature was 30 ℃,and injection volume was 1 μl. RESULTS：The linear range was 0.048-0.480 μg for gallic acid（r=0.999 3）,0.012-0.120 μg for naringin（r=0.999 9）,0.016-0.160 μg for hesperidin（r=0.999 8）,0.022-0.220 μg for neohesperidin（r=0.999 9）and 0.072-0.720 μg for baicalin（r=0.999 2）;limit of quantitation was 2.4,1.6,1.8,1.8,1.6 ng,limit of detection was 7.5,5.0,5.6,5.6,5.0 ng;RSDs of precision,stability and reproducibility tests were no lower than 3.0%;recoveries were 96.64%-102.02%（RSD=2.00%,n=6）,95.86%-102.56%（RSD=2.86%,n=6）,97.24%-102.54%（RSD=2.10%,n=6）,97.44%-102.60%（RSD=2.40%,n=6）and 96.91%-103.13%（RSD=2.62%,n=6）. CONCLUSIONS：The method is rapid and accurate,and can be used for the simultaneous determination of gallic acid,naringin,hesperidin,neohesperidin and baicalin in Qinghou liyan granule.