毛细管电色谱测定复方丹参注射液中原儿茶醛和原儿茶酸的含量

 目的 建立毛细管电色谱分离测定复方丹参注射液中原儿茶醛(PAH)和原儿茶酸(PA)的内标定量测定方法。方法 用ODS柱为固定相,甲醇和2 mmol·L^-1磷酸缓冲液(pH 3.0)为流动相,电压为-8kV,流速为10μL·min^-1,压力为6766.59kPa,紫外检测波长为255 nm,4-羟基苯甲酸为内标。结果 原儿茶醛和原儿茶酸的线性范围分别是0.2-2.5ng和0.042-0.52 ng;相关系数分别为0.999 96和0.999 97;加样回收率分别为98.02%(RSD=3.42％)和100.0％(RSD)=0.93％);检测限分别为0.085 ng和0.036 ng;精密度实验RSD分别为0.52％和0.33％;重现性实验RSD分别为0.27％和0.34％;稳定性实验RSD分别为0.37％和0.32％:柱效分别为113246和257901;PA与PAH的分离度为4.854,PAH与4-羟基苯甲酸的分离度为4.620。结论 该方法简便,快速,准确,灵敏度高,重现性好,样品用量少,适用于丹参及含丹参制剂的样品中原儿茶醛和原儿茶酸的分离测定。

Quantitative determination of protocatechuic aldehyde and protocatechuic acid in compound Danshen injection by capillary electrochromatography

OBJECTIVE To develop a method for the quantitative determination of protocatechuic aldehyde (PAH) and protocatechuic acid (PA) in Compound Danshen Injection by capillary electrochromatography. METHODS Stationary phase was ODS. The mobile phase was composed of methanol and 2 mmol·L^-1 H₃PO₄ buffer solution at pH 3.0. The voltage was at-8 kV. The flow rate was 10μL·min^-1. Pressure was 6766.59 kPa and UV detection wavelength was 255 run. The internal standard was 4-hydrobenzoic acid. RESULTS The linearity ranges of PAH and PA were 0.2-2.5 ng and 0.042-0.52 ng respectively. The correlation coefficients were 0.999 96 and 0.999 97 respectively. The average recoveries of spiked sample were 98.02% (RSD=3.34%) and 99.94% (RSD = 0.91%) respectively. The detection limits were 0.085 ng and 0.036 ng respectively. The RSD (n=5) of intra-batch variation were 0.52% and 0.33% respectively. The RSD (n-5) of inter-batch variation were 0.27% and 0.34% . The RSD of stability were 0.37% and 0.32% respectively. The column efficiencies per meter were 113 246 and 257 901 respectively. The resolution between PA and PAH was 4.854 and the resolution between PAH and 4-hydrobenzoic acid was 4.620. CONCLUSION The method was simple, rapid, accurate, sensitive and reproducible with small sample consuming. It is suitable for the determination of PAH and PA in Danshen and Danshen preparations.