论文部分内容阅读
目的:建立测定氟比洛芬酯原料药中镍残留量的方法。方法:采用火焰原子吸收分光光度法,样品用无水乙醇溶解后直接测定。测定波长为232.0 nm,灯电流为12 m A,乙炔流量为1.6 L/min,空气流量为15 L/min,狭缝宽为0.2 nm,燃烧器高度为7mm。结果:镍检测质量浓度线性范围为0~3μg/ml(r=0.998 4);检测限为0.03μg/ml;精密度、重复性试验的RSD<1%;加样回收率为96.81%~100.90%,RSD=1.3%(n=9)。结论:该方法操作简便、精密度好,结果准确、可靠,适用于测定氟比洛芬酯原料药中镍的残留量。
Objective: To establish a method for the determination of nickel residues in flurbiprofen ester raw materials. Methods: Flame atomic absorption spectrophotometry was used. The sample was directly dissolved in anhydrous ethanol. The measurement wavelength was 232.0 nm, the lamp current was 12 m A, the acetylene flow rate was 1.6 L / min, the air flow rate was 15 L / min, the slit width was 0.2 nm and the burner height was 7 mm. Results: The linear range of nickel detection was 0 ~ 3μg / ml (r = 0.998 4), the detection limit was 0.03μg / ml, the RSD of precision and repeatability test was less than 1%, the recoveries were 96.81% ~ 100.90 %, RSD = 1.3% (n = 9). Conclusion: The method is simple, accurate, accurate and reliable. It is suitable for the determination of nickel residues in flurbiprofen ester raw materials.