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目的:建立同时测定糖肾清毒颗粒中7种活性成分含量的方法。方法:采用高效液相色谱法。色谱柱为岛津Inert Sustain C18,流动相为乙腈-0.1%磷酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长为327 nm(绿原酸和咖啡酸)、280 nm(黄芩苷)、228 nm(牛蒡苷)、276 nm(汉黄芩苷、黄芩素和汉黄芩素),柱温为35 ℃,进样量为10 μL。结果:绿原酸、咖啡酸、黄芩苷、牛蒡苷、汉黄芩苷、黄芩素和汉黄芩素检测质量浓度线性范围分别为4.830~154.6 μg/mL(r=0.999 8)、0.750~24.1 μg/mL(r=0.999 7)、22.859~731.5 μg/mL(r=0.999 7)、8.491~271.7 μg/mL(r=0.999 3)、2.471~79.0 μg/mL(r=0.999 6)、6.656~213.0 μg/mL(r=0.999 4)、2.756~88.2 μg/mL(r=0.999 8);精密性、稳定性、重复性的RSD<2.0%;加样回收率分别为96.86%~100.82%(RSD=1.46%,n=6)、98.79%~101.09%(RSD=0.93%,n=6)、97.57%~101.51%(RSD=1.37%,n=6)、97.76%~99.63%(RSD=0.77%,n=6)、97.99%~100.12%(RSD=0.76%,n=6)、96.54%~101.07%(RSD=1.87%,n=6)、96.60%~99.59%(RSD=1.14%,n=6)。结论:该方法操作简便,精密度、稳定性、重复性好,可用于糖肾清毒颗粒中7种活性成分含量的同时测定。
OBJECTIVE: To establish a method for the simultaneous determination of 7 active constituents in Tangshen qingdu granule. METHODS: HPLC was performed on the column of SHIMADZU Inert Sustain C18 with mobile phase of acetonitrile- 0.1% phosphoric acid at a flow rate of 1.0 mL/min, detection wavelength was 327 nm for chlorogenic acid and caffeic acid, 280 nm for baicalin, 228 nm for arctiin and 276 nm for wogonoside, baicalein and wogonin, column temperature was 35 ℃, and injection volume was 10 μL. RESULTS: The linear range was 4.830-154.6 μg/mL for chlorogenic acid and (r=0.999 8), 0.750-24.1 μg/mL for caffeic acid(r=0.999 7),22.859-731.5 μg/mL for baicalin(r=0.999 7),8.491-271.7 μg/mL for arctiin (r=0.999 3), 2.471-79.0 μg/mL for wogonoside(r=0.999 6),6.656-213.0 μg/mL for baicalein(r=0.999 4) and 2.756-88.2 μg/mL for wogonin (r=0.999 8); RSDs of precision, stability and reproducibility tests were lower than 2.0%, recoveries were 96.86%-100.82% (RSD=1.46%,n=6), 98.79%-101.09%(RSD=0.93%,n=6), 97.57%-101.51%(RSD=1.37%,n=6), 97.76%-99.63% (RSD=0.77%,n=6), 97.99%-100.12%(RSD=0.76%,n=6), 96.54%-101.07%(RSD=1.87%,n=6) and 96.60%-99.59% (RSD=1.14%,n=6). CONCLUSIONS: The method is simple with good precision, stability and reproducibilty, and can be used for the simultaneous determination of 7 active constituents in Tangshen qingdu granule.
高效液相色谱法糖肾清毒颗粒黄芩黄酮类牛蒡苷含量测定
HPLC?Tangshen?qingdu?granule?BaicalinFlavonidArctiinContent determination
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