电感耦合等离子体质谱法检测盐酸赖氨酸与醋酸赖氨酸原料药中11种元素杂质OA

Objective To establish an inductively coupled plasma-mass spectrometry(ICP-MS)method for the content determination of the 11 elemental impurities[cadmium(Cd),lead(Pb),arsenic(As),mercury(Hg),cobalt(Co),alum(V),nickel(Ni),lithium(Li),antimony(Sb),copper(Cu),and aluminum(Al)]in lysine hydrochloride and lysine acetate active pharmaceutical ingredients(APIs).Methods The sample was directly dissolved in the 2%dilute nitric acid solution,the plasma power was 1 550 W,the plasma gas flow rate was 14.0 L/min,the carrier gas flow rate was 4.9 L/min,the collision gas flow rate was 4.3 mL/min,the atomization chamber temperature was 2.7℃,the peristaltic pump speed was 40 r/min,and the detection mode was kinetic energy discrimination(KED).Results The 11 elements had good linear relationship with their response count values within their respective mass concentration ranges(r>0.996,n=5).The RSDs of repeatability and intermediate precision tests were lower than 3%,and the recovery rate of the test solution was in the range of 90.0%-110.0%,with an RSD<3.0%(n=9).The detection levels of the above 11 elemental impurities in each batch of lysine hydrochloride and lysine acetate samples were all lower than their respective control limits.Conclusion This method has fast analysis speed,good specificity,high sensitivity and accuracy,which can be used for the detection of 11 elemental impurities in lysine hydrochloride and lysine acetate APIs.