摘要
目的建立同时测定头孢呋辛酯片中1类元素铅(Pb)、镉(Cd)、砷(As)、汞(Hg)和2A类元素钴(Co)、钒(V)、镍(Ni)7种元素杂质含量的电感耦合等离子体质谱法。方法样品经硝酸微波消解。以72Ge,115In,209Bi为内标,测定模式为氦气模式,等离子体模式为通用模式,等离子气体、载气、辅助气、氦气流量分别为15,1,0.9,4.3 L/min,采样深度为10.0 mm,蠕动泵转速为0.3 r/s,雾化室温度为2℃。结果V,Co,Ni,As,Cd,Hg,Pb 7种元素杂质在限度浓度的10%~200%范围内与其响应值和内标响应值的比值线性关系良好(r>0.998);检测限为0.25~30.50 ng/g,定量限为0.75~91.52 ng/g(n=10);精密度试验结果的RSD均小于3.0%(n=6);加样回收率分别为105.04%,101.96%,100.93%,103.44%,103.73%,106.03%,106.61%,RSD分别为1.03%,1.08%,1.24%,1.63%,1.10%,2.69%,3.58%(n=9)。3批样品中,7种元素杂质的含量均小于限度浓度的10%。结论该方法灵敏度高、准确度和精密度良好,可用于头孢呋辛酯片中1类和2A类7种元素杂质的含量测定。头孢呋辛酯片中7种元素杂质无残留风险。
Objective To establish an inductively coupled plasma-mass spectrometry method for the simultaneous determination of Class 1 elemental impurities[lead(Pb),cadmium(Cd),arsenic(AS),mercury(Hg)],and Class 2A elemental impurities[cobalt(Co),vanadium(V),and nickel(Ni)]in Cefuroxime Axetil Tablets.Methods The sample was acidified with nitric acid and digested with microwave.With 72Ge,115In,and 209Bi as internal standards,the determination mode was helium(He)mode,and the plasma mode was general mode.The flow rates of plasma gas,carrier gas,auxiliary gas,and helium gas were 15,1,0.9,and 4.3 L/min,respectively.The sampling depth was 10.0 mm,the peristaltic pump speed was 0.3 r/s,and the atomization chamber temperature was 2℃.Results The linear range of V,Co,Ni,As,Cd,Hg,and Pb was 10%-200%(r>0.998).The limit of detection was in the range of 0.25-30.50 ng/g,and the limit of quantification was in the range of 0.75-91.52 ng/g(n=10).The RSD of the precision test was lower than 3.0%(n=6).The recoveries of V,Co,Ni,As,Cd,Hg,and Pb were 105.04%,101.96%,100.93%,103.44%,103.73%,106.03%,and 106.61%,with RSDs of 1.03%,1.08%,1.24%,1.63%,1.10%,2.69%,and 3.58%(n=9),respectively.In the three batches of samples,the content of seven elemental impurities was lower than 10%of the limit concentration.Conclusion This method has high sensitivity,good accuracy,and precision,and can be used for the determination of seven elemental impurities(Class 1 and Class 2A elemental impurities)in Cefuroxime Axetil Tablets.There is no residual risk of seven elemental impurities in Cefuroxime Axetil Tablets.
作者
刘翠
LIU Cui(Zhuhai United Laboratory Zhongshan Co.,Ltd.,Zhongshan,Guangdong,China 528467)
出处
《中国药业》
CAS
2024年第21期84-87,共4页
China Pharmaceuticals
基金
广东省中山市健康医药产业发展专项资金项目[中工信〔2019〕553号]。
