HPLC同时测定斑蝥酸钠维生素B6注射液中斑蝥酸钠和维生素B6的含量

Simultaneous Determination of Disodium Cantharidinate and Vitamin B6 in Disodium Cantharidinate and Vitamin B6 Injection by HPLC

关键词:  斑蝥酸钠维生素B₆注射液  斑蝥酸钠  维生素B₆  高效液相色谱法  含量测定

Key words:  Disodium Cantharidinate and Vitamin B₆ injection  disodium cantharidinate  vitamin B₆  HPLC  quantitative analysis

摘要:

目的 建立斑蝥酸钠维生素B₆注射液中斑蝥酸钠和维生素B₆含量的同时测定方法。方法 采用HPLC，色谱柱为Syncronis C₁₈（250 mm×4.6 mm，5 μm），流动相为0.02 mol·L^-1磷酸二氢钾溶液（磷酸调pH值至2.6）-乙腈，梯度洗脱，流速为1.0 mL·min^-1，检测波长为193，290 nm，波长切换法，柱温：30℃。结果 斑蝥酸钠回归方程为Y=1.926X+0.010（r=0.999 7），在0.064 6~0.322 8 mg·mL^-1内斑蝥酸钠与峰面积的线性关系良好，平均回收率为98.9%，RSD为1.2%（n=9）。维生素B₆回归方程为Y=24.153X+0.670（r=0.999 9），在0.535 9~2.679 7 mg·mL^-1内维生素B₆与峰面积的线性关系良好，平均回收率为100.2%，RSD为1.0%（n=9）；仪器精密度、稳定性和重复性试验的RSD均<2.0%。结论 所建立的方法结果准确、重复性好，可用于斑蝥酸钠维生素B₆注射液的质量控制。

Abstract:

OBJECTIVE To establish method for simultaneous determination of disodium cantharidinate and vitamin B₆ in Disodium Cantharidinate and Vitamin B₆ injection. METHODS HPLC was performed on a Syncronis C₁₈ column(250 mm×4.6 mm, 5 μm) using the gradient 0.02 mol·L^-1 potassium phosphate monobasic solution(adjust pH to 2.6 with H₃PO₄)(A)-acetonitrile(B) at the 1.0 mL·min^-1 flow rate as mobile phase. The column temperature was 30℃ and the detection wavelengths were 193 nm and 290 nm(wavelength switching). RESULTS The linear regression equation of disodium cantharidinate was Y=1.926X+0.010(r=0.999 7); the linear range was 0.064 6-0.322 8 mg·mL^-1 with the average recovery of 98.9% and the RSD of 1.2%(n=9). The linear regression equation of vitamin B₆ was Y=24.153X+0.670(r=0.999 9); the linear range was 0.535 9-2.679 7 mg·mL^-1 with the average recovery of 100.2% and the RSD of 1.0%(n=9). The RSD values for the instrument precision, stability and repeatability were all <2.0%. CONCLUSION The established HPLC method appears to be accurate and reproducible, which can be used for the quality control of Disodium Cantharidinate and Vitamin B₆ injection.