电感耦合等离子体质谱(ICP-MS)法测定人凝血因子Ⅷ/血管性血友病因子复合物冻干注射剂中的21种元素

Determination of 21 elements in Human Coagulation FactorⅧ/von Willebrand Factor Complex Lyophilized Injection by ICP-MS

目的建立电感耦合等离子体质谱(ICP-MS)同时测定人凝血因子Ⅷ/血管性血友病因子复合物冻干注射剂中硼(B)、镁(Mg)、铝(Al)、硅(Si)、钒(V)、镉(Cr)、锰(Mn)、铁(Fe)、钴(Co)、镍(Ni)、铜(Cu)、锌(Zn)、锶(Sr)、锆(Zr)、钼(Mo)、铑(Rh)、钯(Pd)、锡(Sn)、钡(Ba)、铈(Ce)、铅(Pb)元素含量的方法。方法样品经微波消解后,以钪(Sc)、锗(Ge)、铟(In)、铋(Bi)为内标,采用电感耦合等离子体质谱(ICP-MS)法同时测定上述元素的含量。ICP-MS功率为1550 W,采样深度为10.0 mm,等离子气、雾化气、辅助气流量分别为15.0、0.99、0.9 L·min^(-1),泵速为0.10 r·s^(-1),雾化室温度为2℃,硼(B)元素采用No Gas调谐模式,其他元素采用He调谐模式,数据采集3次。结果21种元素在测定的浓度范围内,线性关系良好,相关系数r>0.9990;检出限为0.001~2.04μg·L^(-1);各元素回收率为87.78%~102.72%,RSD为1.31%~7.91%。结论该方法快速简便、灵敏度高、准确性好,可用于人凝血因子Ⅷ/血管性血友病因子复合物冻干注射剂中金属元素的检测。

Objective To establish an inductively coupled plasma mass spectrometry(ICP-MS)method for the simultaneous determination of boron(B),magnesium(Mg),aluminum(Al),silicon(Si),vanadium(V),cadmium(Cr),manganese(Mn),iron(Fe),cobalt(Co),nickel(Ni),copper(Cu),zinc(Zn),strontium(Sr),zirconium(Zr),molybdenum(Mo),rhodium(Rh),palladium(Pd),tin(Sn),barium(Ba),cerium(Ce)and lead(Pb)in human coagulation factorⅧ/von Willebrand factor complex lyophilized injection.Methods After microwave digestion of samples,with scandium(Sc),germanium(Ge),indium(In)and bismuth(Bi)as internal standard,the content of the above elements were determined by inductively coupled plasma mass spectrometry(ICP-MS)method at the same time,the ICP-MS power was 1550 W,sampling depth was 10.0 mm,plasma gas,carrier gas and auxiliary gas flow were 15.0,0.99,0.9 L·min^(-1) respectively,the pump speed was 0.10 r·s^(-1),the atomizing chamber temperature was 2℃,reaction mode was No Gas(B)and helium(others),data was collected for three times.Results The 21 elements have a good linear relationship within the measured concentration range,the correlation coefficient r>0.999;the detection limit was 0.001~2.04μg·L^(-1);the recoveries of each element were 87.78%~102.72%,and the RSDs were 1.31%~7.91%.Conclusion The method was rapid,simple,sensitive and accurate,and can be used for the detection of metal elements in freeze-dried injections of human coagulation factorⅧ/von Willebrand factor complex.