ICP-MS法同时测定广西白背叶药材中30种微量元素的含量

Content Determination of 30 Kinds of Microelements in Mallotus apelta from Guangxi by ICP-MS

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1 550 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 m L/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10～1 000 ng/mL(r=0.999 9)、0.1～5 ng/mL(r=0.999 9)、0.1～5 ng/mL(r=0.999 9)、10～1 000 ng/mL(r=0.999 9)、10～1 000 ng/mL(r=0.999 9)、0.1～5 ng/mL(r=0.999 7)、0.5～100 ng/mL(r=0.999 7)、1～500 ng/mL(r=0.999 8)、1～100 ng/mL(r=0.999 7)、0.5～50 ng/mL(r=0.999 9)、0.5～50 ng/mL(r=0.999 9)、0.1～10 ng/mL(r=0.999 9)、0.1～10 ng/mL(r=0.999 9)、0.1～10 ng/mL(r=0.999 9)、0.1～10 ng/mL(r=0.999 9)、1～500 ng/mL(r=0.999 9)、0.1～10 ng/mL(r=0.999 9)、0.1～10 ng/mL(r=0.999 9)、0.1～10 ng/mL(r=0.999 9)、0.1～10 ng/mL(r=0.999 8)、0.1～10 ng/mL(r=0.999 9)、0.1～10 ng/mL(r=0.999 9)、0.1～10 ng/mL(r=0.999 9)、0.1～10 ng/mL(r=0.999 9)、0.1～10 ng/mL(r=0.999 9)、0.1～10 ng/mL(r=0.999 8)、0.1～5 ng/mL(r=0.998 4)、0.1～10 ng/mL(r=0.999 9)、0.5～100 ng/mL(r=0.999 7)、0.1～10 ng/mL(r=0.999 9),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。

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 1 550 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 10-1 000 ng/mL（r=0.999 9）, 0.1-5 ng/mL（r=0.999 9）, 0.1-5 ng/mL（r=0.999 9）, 10-1 000 ng/mL （r=0.999 9）, 10-1000 ng/mL（r=0.999 9）,0.1-5 ng/mL（r=0.999 7）, 0.5-100 ng/mL（r=0.999 7）, 1-500 ng/mL（r=0.999 8）, 1-100 ng/mL（r=0.999 7）, 0.5-50 ng/mL（r=0.999 9）, 0.5-50 ng/mL（r=0.999 9）, 0.1-10 ng/mL（r=0.999 9）, 0.1-10 ng/mL（r= 0.999 9）, 0.1-10 ng/mL（r=0.999 9）, 0.1-10 ng/mL（r=0.999 9）, 1-500 ng/mL（r=0.999 9）, 0.1-10 ng/mL（r=0.999 9）, 0.1-10 ng/mL（r=0.999 9）,0.1-10 ng/mL（r=0.999 9）, 0.1-10 ng/mL（r=0.999 8）, 0.1-10 ng/mL（r=0.999 9）,0.1-10 ng/mL（r=0.999 9）, 0.1-10 ng/mL（r=0.999 9）,0.1-10 ng/mL（r=0.999 9）, 0.1-10 ng/mL（r=0.999 9）, 0.1-10 ng/mL（r=0.999 8）, 0.1-5 ng/mL（r= 0.998 4）,0.1-10 ng/mL（r=0.999 9）,0.5-100 ng/mL（r=0.999 7）,0.1-10 ng/mL（r=0.999 9）, respectively. The limits of quantitation 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 A1 in samples were the highest. CONCLUSIONS： The method is simple, precise, stable and reproducible, 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.