在线固相萃取技术在肝肾滋糖浆剂甜菜碱含量测定中的应用研究

Application of online solid phase extraction technology in the determination of betaine content in ganshenzi syrup

建立在线固相萃取技术结合高效液相色谱法测定肝肾滋糖浆剂中甜菜碱含量的方法。利用双三元液相色谱系统,经阳离子交换柱(50×4 mm,5μm)进行在线固相萃取,使用氨基柱(250×4.6 mm,5μm)分离目标组分,以乙腈为流动相A、0.1%磷酸水为流动相B、梯度洗脱,检测波长190 nm,柱温30℃,流速为1.0 mL·min^(-1),进样量为10μL。甜菜碱浓度在0.04294~1.0306 mg·mL^(-1)范围内线性关系良好(r=0.9999),供试品溶液在室温下8 h内基本稳定,重现性试验的平均含量为4.1303 mg·g^(-1)、RSD为1.4%,准确度试验的平均加样回收率为94.93%、RSD为1.5%,高低浓度水平样品的平均加样回收率和RSD分别为100.7%、96.96%、2.2%、1.9%。该方法快速简便、准确度高、稳定性好、范围宽,适用于肝肾滋糖浆剂中甜菜碱的含量测定,可为提升肝肾滋质量标准提供技术支持。

To establish an on-line solid phase extraction(SPE)couple with high performance liquid chromatography(HPLC)method for the determination of betaine content in Ganshenzi syrup.On-line solid phase extraction was performed using a dual-gradient liquid chromatography system with a cation exchange column(50×4 mm,5μm),and the target components were separated using an a-mino column(250×4.6 mm,5μm).The target components were separated by acetonitrile as mobile phase A and water(containing 0.1%phosphoric acid)as mobile phase B,eluted by equal gradient,the detection wavelength was 190 nm,the column temperature was 30°C,the flow rate was 1.0 mL·min^(-1),and the injection volume was 10μL.The linearity of betaine concentration was good in the range of 0.04294~1.0306 mg·mL^(-1)(r=0.9999),the sample solution were stable within 8 hour at room temperature,the average content of reproducibility test was 4.1303 mg·g^(-1),RSD was 1.4%,the average recovery of accuracy test was 94.93%,RSD was 1.5%.The average recoveries of high concentration and low concentration samples were 100.7%and 97.0%,RSDs were2.2%and 1.9%.The method is rapid,simple,accurate,stable and wide in range.It is suitable for the determination of betaine content in Ganshenzi syrup and can provide technical support for improving the quality standard of Ganshenzi.