ICP-MS法同时测定广西白背叶药材中30种微量元素的含量

摘要

OBJECTIVE:To establish a method for simultaneous determination of 30 kinds of microelements in Mallotus apelta from Guangxi. METHODS:ICP-MS method was adopted. The radio frequency power was 1550 W,the sampling depth was 10 mm,the carrier gas velocity was 1.05 L/min,the atomizing chamber temperature was 2 ℃,and the peristaltic pump was 0.10 rps. The collision mode was He,and the gas flow rate was 4.2 mL/min. RESULTS:The linear ranges of aluminum,vanadium,chromi-um,manganese,iron,nickel,copper,zinc,gallium,arsenic,cadmium,antimony,molybdenum,rubidium,cesium,barium, lanthanum,cerium,praseodymium,neodymium,europium,gadolinium,dysprosium,holmium,erbium,lutetium,mercury,thal-lium,lead and uranium were 10-1000 ng/mL(r=0.9999),0.1-5 ng/mL(r=0.9999),0.1-5 ng/mL(r=0.9999),10-1000 ng/mL (r=0.9999),10-1000 ng/mL(r=0.9999),0.1-5 ng/mL(r=0.9997),0.5-100 ng/mL(r=0.9997),1-500 ng/mL(r=0.9998), 1-100 ng/mL(r=0.9997),0.5-50 ng/mL(r=0.9999),0.5-50 ng/mL(r=0.9999),0.1-10 ng/mL(r=0.9999),0.1-10 ng/mL(r=0.9999),0.1-10 ng/mL(r=0.9999),0.1-10 ng/mL(r=0.9999),1-500 ng/mL(r=0.9999),0.1-10 ng/mL(r=0.9999),0.1-10 ng/mL(r=0.9999),0.1-10 ng/mL(r=0.9999),0.1-10 ng/mL(r=0.9998),0.1-10 ng/mL(r=0.9999),0.1-10 ng/mL(r=0.9999), 0.1-10 ng/mL(r=0.9999),0.1-10 ng/mL(r=0.9999),0.1-10 ng/mL(r=0.9999),0.1-10 ng/mL(r=0.9998),0.1-5 ng/mL(r=0.9984),0.1-10 ng/mL(r=0.9999),0.5-100 ng/mL(r=0.9997),0.1-10 ng/mL(r=0.9999),respectively. The limits of quantita-tion were no higher than 0.44 mg/kg,and the limits of detection were no higher than 0.11 mg/kg. RSDs of precision,stability and reproducibility tests were no more than 10.0%. The recoveries were 80.45%-116.68%(RSD ranged 0.47%-5.83%,n=6). The con-tents of Mn,Ba Fe and Al in samples were the highest. CONCLUSIONS:The method is simple,precise,stable and reproduc-ible,and can be used for simultaneous determination of 30 kinds of microelements in M. apelta from Guangxi. The contents of harmful elements are in line with national standard.%目的:建立同时测定广西白背叶药材中30种微量元素含量的方法.方法:采用电感耦合等离子体质谱法.射频功率为1550 W,采样深度为10 mm,载气流速为1.05 L/min,雾化室温度为2℃,蠕动泵频率为0.10 rps,碰撞模式为氦,气流量为4.2 mL/min.结果:铝、钒、铬、锰、铁、镍、铜、锌、镓、砷、铷、钼、镉、锑、铯、钡、镧、铈、镨、钕、铕、钆、镝、钬、铒、镥、汞、铊、铅、铀检测质量浓度线性范围分别为10~1000 ng/mL(r=0.9999)、0.1~5 ng/mL(r=0.9999)、0.1~5 ng/mL(r=0.9999)、10~1000 ng/mL(r=0.9999)、10~1000 ng/mL(r=0.9999)、0.1~5 ng/mL(r=0.9997)、0.5~100 ng/mL(r=0.9997)、1~500 ng/mL(r=0.9998)、1~100 ng/mL(r=0.9997)、0.5~50 ng/mL(r=0.9999)、0.5~50 ng/mL(r=0.9999)、0.1~10 ng/mL(r=0.9999)、0.1~10 ng/mL(r=0.9999)、0.1~10 ng/mL(r=0.9999)、0.1~10 ng/mL(r=0.9999)、1~500 ng/mL(r=0.9999)、0.1~10 ng/mL(r=0.9999)、0.1~10 ng/mL(r=0.9999)、0.1~10 ng/mL(r=0.9999)、0.1~10 ng/mL(r=0.9998)、0.1~10 ng/mL(r=0.9999)、0.1~10 ng/mL(r=0.9999)、0.1~10 ng/mL(r=0.9999)、0.1~10 ng/mL(r=0.9999)、0.1~10 ng/mL(r=0.9999)、0.1~10 ng/mL(r=0.9998)、0.1~5 ng/mL(r=0.9984)、0.1~10 ng/mL(r=0.9999)、0.5~100 ng/mL(r=0.9997)、0.1~10 ng/mL(r=0.9999),定量限≤0.44 mg/kg,检测限≤0.11 mg/kg;精密度、稳定性、重复性试验的RSD≤10.0%;加样回收率为80.45%~116.68%(RSD为0.47%~5.83%,n=6).药材样品中Mn、Ba、Fe、Al的含量最高.结论:该方法操作简便,精密度、稳定性、重复性好,可用于广西白背叶药材中30种微量元素含量的同时测定;药材中有害元素的含量符合国家相关标准.