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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。
Objective To establish a quantitative method for the determination of protocatechuic aldehyde (PAH) and protocatechuic acid (PA) in compound Danshen injection by capillary electrochromatography. Methods ODS column was used as stationary phase, methanol and 2 mmol·L-1 phosphate buffer (pH 3.0) as mobile phase, voltage was -8kV, flow rate was 10μL·min-1, pressure was 6676.59kPa, UV detection wavelength was 255. Nm, 4-hydroxybenzoic acid is an internal standard. Results The linear ranges of protocatechuic aldehyde and protocatechuic acid 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 recoveries were 98.02% (RSD=3.42%) and 100.0% (RSD) = 0.93%); the detection limits were 0.085 ng and 0.036 ng, respectively; precision test RSDs were 0.52% and 0.33%, reproducibility experiments RSD were 0.27% and 0.34%, respectively; stability test RSD were The results were 0.37% and 0.32%: the column efficiency was 113246 and 257901 respectively; the separation degree between PA and PAH was 4.854, and the degree of separation between PAH and 4-hydroxybenzoic acid was 4.620. Conclusion The method is simple, rapid, accurate, sensitive, reproducible, and less in sample. It is suitable for the separation and determination of protocatechuic aldehyde and protocatechuic acid in samples of Salvia miltiorrhiza and Salvia miltiorrhiza.