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目的:建立同时测定参柏舒心颗粒中丹参素钠、原儿茶醛、丹酚酸 B和盐酸黄柏碱含量的方法。方法:采用高效液相色谱法。色谱柱为Waters sunfire-C18,流动相为乙腈-0.05%三氟乙酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长为288 nm,柱温为30 ℃,进样量为5 μL。结果:丹参素钠、原儿茶醛、丹酚酸 B和盐酸黄柏碱检测进样量线性范围分别为0.040 01~1.600 46 μg(r=0.999 9)、0.013 84~0.553 7 μg(r=0.999 9)、0.049 32~1.972 94 μg(r=0.999 6)、0.014 46~0.578 6 μg(r=0.999 8);定量限分别为7.68、2.66、4.74、1.38 ng,检测限分别为1.92、0.66、2.36、0.69 ng;精密度、稳定性、重复性试验的RSD<2%;加样回收率分别为98.846%~100.762%(RSD=0.77%,n=6)、96.632%~99.463%(RSD=0.98%,n=6)、98.541%~100.432%(RSD=0.82%,n=6)、98.607%~101.521%(RSD=1.11%,n=6)。结论: 该方法操作简便、结果准确、精密度好,可用于参柏舒心颗粒中4种成分含量的同时测定。
OBJECTIVE: To establish a method for simultaneous determination of sodium danshensu, protocatechuic aldehyde, salvianolic acid B and phellodendrine hydrochloride in Shenbai shuxin granules. METHODS: HPLC method was adopted. The separation was performed on Waters sunfire-C18 column with mobile phase consisted of acetonitrile-0.05% trifluoroacetic acid (gradient elution) at the flow rate of 1.0 mL/min. The detection wavelength was set at 288 nm, and the column temperature was 30 ℃. The sample size was 5 μL. RESULTS: The linear ranges of sodium danshensu, protocatechuic aldehyde, salvianolic acid B and phellodendrine hydrochloride were 0.040 01-1.600 46 μg(r=0.999 9),0.013 84-0.553 7 μg(r=0.999 9),0.049 32-1.972 94 μg(r=0.999 6), 0.014 46-0.578 6 μg(r=0.999 8). The limits of quantitation were 7.68, 2.66, 4.74, 1.38 ng, and the limits of detection were 1.92,0.66, 2.36, 0.69 ng, respectively. RSDs of precision, stability and reproducibility tests were all lower than 2%. The recoveries were 98.846%-100.762%(RSD=0.77%,n=6), 96.632%-99.463%(RSD=0.98%,n=6), 98.541%-100.432%(RSD=0.82%,n=6), 98.607%-101.521%(RSD=1.11%,n=6), respectively. CONCLUSIONS: The method is simple, accurate and precise. It can be used for 4 components in Shenbai shuxin granules.
参柏舒心颗粒含量测定丹参素钠原儿茶醛丹酚酸 B盐酸黄柏碱高效液相色谱法
Shenbai shuxin granulesContent determinationSodium danshensuProtocatechuic aldehydeSalvianolic acid BPhellodendrine hydrochlorideHPLC
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