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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 C18,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1 μl。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0.048~0.480 μg(r=0.999 3)、0.012~0.120 μg(r=0.999 9)、0.016~0.160 μg(r=0.999 8)、0.022~0.220 μg(r=0.999 9)、0.072~0.720 μg(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 C18 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.
超高效液相色谱法清喉利咽颗粒没食子酸橙皮苷新橙皮苷柚皮苷黄芩苷
UPLCQinghou liyan granuleGallic acidNaringinHesperidinNeohesperidinBaicalin
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