论文部分内容阅读
目的用HPLC法验证原有测定枸橼酸钾溶液中枸橼酸钾和羟苯乙酯含量的方法,并与原方法进行比对。方法采用Nucleodur C18Pyramid(250 mm×4.6 mm,5μm)色谱柱。梯度洗脱,流动相A:水-磷酸(1000∶1);流动相B:乙腈。洗脱程序:0~5 min,A100%;5.01~22 min:A70%,B30%;22.1~30 min,A100%;流速1 ml·min-1,检测波长210 nm。结果以峰面积(Y)对进样浓度(X,μg·ml-1)进行线性回归,枸橼酸钾回归方程为Y=2.586 X-16.49,r=0.9999,线性范围500.8~5008μg·ml-1;羟苯乙酯回归方程为Y=0.021 44 X-0.4065,r=0.9999,线性范围2.503~25.03μg·ml-1;枸橼酸钾回收率为100.2%,RSD为0.15%;羟苯乙酯回收率为99.6%,RSD为1.9%。结论 HPLC法测定结果准确,重复性好,操作简便,优于原方法,可更好的用于枸橼酸钾溶液中枸橼酸钾和羟苯乙酯的含量测定。
Objective To verify the original method for the determination of potassium citrate and hydroxyphenylethyl ester in potassium citrate solution by HPLC and to compare with the original method. Methods Nucleodur C18 Pyramid (250 mm × 4.6 mm, 5 μm) was used. Gradient elution, mobile phase A: water-phosphoric acid (1000: 1); Mobile phase B: acetonitrile. Elution program: 0 ~ 5 min, A100%; 5.01 ~ 22 min: A70%, B30%; 22.1 ~ 30 min, A100%; flow rate 1 ml · min- 1, detection wavelength 210 nm. Results The regression equation of the concentration of potassium citrate was Y = 2.586 X-16.49, r = 0.9999. The linear range was 500.8-5008μg · ml-1. 1; the regression equation of hydroxyacetophenone is Y = 0.021 44 X-0.4065, r = 0.9999, the linear range is 2.503 ~ 25.03 μg · ml-1; the recovery rate of potassium citrate is 100.2% and the RSD is 0.15% The ester recovery was 99.6% with a RSD of 1.9%. Conclusion The HPLC method is accurate, reproducible and simple to operate. It is superior to the original method and can be used for the determination of potassium citrate and phenethyl citrate in potassium citrate solution.