UPLC法同时测定清喉利咽颗粒中5种成分的含量
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篇名: UPLC法同时测定清喉利咽颗粒中5种成分的含量
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摘要: 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。
ABSTRACT: 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.
期刊: 2016年第27卷第30期
作者: 牛小花,陈洪源,段玉平,黄娇
AUTHORS: NIU Xiaohua,CHEN Hongyuan,DUAN Yuping,HUANG Jiao
关键字: 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
KEYWORDS: UPLC; Qinghou liyan granule; Gallic acid; Naringin; Hesperidin; Neohesperidin; Baicalin
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