加校正因子的主成分自身对照法测定维生素B_(6)片中有关物质

Determination of Related Substances in Vitamin B_(6) Tablets by Principal Component Self-control with Correction Factors

目的 建立高效液相色谱-加校正因子的主成分自身对照法测定维生素B_(6)片中杂质A、杂质B、未知最大单杂及杂质总量。方法 采用Inertsil ODS-SP(4.6×250 mm,5μm)色谱柱,以0.04%戊烷磺酸钠溶液(冰醋酸调p H至3.0)-甲醇(92∶8)为流动相,流速为1.0 m L·min^(-1),检测波长为291 nm。结果 维生素B_(6)杂质A和杂质B的校正因子分别为1.4、1.3。维生素B_(6)对照品、杂质A和杂质B分别在(0.4988~24.94)μg·m L^(-1)、(0.5005~5.005)μg·m L^(-1)、(0.5025~5.025)μg·m L^(-1)质量浓度范围内与峰面积呈良好的线性关系(r均为1.000)。杂质A和杂质B检测限分别为0.069μg·m L^(-1)、0.0739μg·m L^(-1)。杂质A、杂质B平均回收率分别为99.98%(RSD=0.56%)、100.02%(RSD=0.79%)。供试品溶液重复性及稳定性均良好。结论 本方法专属性强、灵敏准确,重现性好,可有效控制维生素B_(6)片中的杂质。

OBJECTIVE To establish an HPLC-principal component self-reference with correction factors method for determinating the impurity A,the impurity B,maximum single impurity and total impurity in vitamin B_(6)tablets.METHODS Ultimate Inertsil ODS-SP (4.6×250 mm,5μm) column with 0.04%sodium pentane sulfonate solution (glacial acetic acid adjusted to pH 3.0) and methanol (92∶8) as mobile phase at the flow rate of 1.0 m L·min^(-1).The detection wavelength was set at 291 nm.RESULTS The correction factors of the impurity A and B were1.4 and 1.3.The concentrations of vitamin B_(6),the impurity A and the impurity B were in the range of (0.4988-24.94)μg·mL^(-1),(0.5005-5.005)μg·mL^(-1)and (0.5025-5.025)μg·mL^(-1)(r=1.000).The detection limitsof the impurity A and impurity B were 0.069μg·m L^(-1)and 0.0739μg·m L^(-1),respectively.The average recoveries of the impurity A and the impurity B were 99.98%(RSD=0.56%) and 100.02%(RSD=0.79%).The tested solution had good repeatability and stability.CONCLUSION The method is specific,sensitive,accurate and reproducible,and can effectively control the impurities in vitamin B_(6)tablets.