ICP-MS法同时测定白石脂药材中27种重金属及微量元素的含量

Simultaneous Determination of 27 Kinds of Heavy Metals and Trace Elements in Halloysitum album by ICP-MS

目的:建立同时测定不同产地白石脂药材中27种重金属及微量元素含量的方法。方法:样品经湿法消解后,采用电感耦合等离子体质谱法进行测定。载气为氩气,碰撞气为氦气,等离子体气流速为15.0 L/min,载气流速为1.17 L/min,碰撞气体流量为5.0 mL/min,雾化器为Barbinton,采样深度为8.0 mm,雾化室温度为2℃,等离子体射频功率为1.3 kW,蠕动泵转数为30 r/min;采用全定量分析模式,测点数为3,分析时间为0.1 s,重复3次。采用PASW Statistics 18.0软件进行聚类分析。结果:27种重金属及微量元素检测质量浓度的线性范围为0～200μg/L(r≥0.996 5);定量限为0.003 41～75.485μg/L,检测限为0.001 1～24.350 0μg/L;精密度、稳定性、重复性试验的RSD均小于7%;平均加样回收率为72.3%～129.1%,RSD为0.9%～9.4%(n=6);铝含量为0.01～123 220.20 mg/kg,铝是含量最高的元素,锂、钠、镁、钾、钙、钒、锰、铁、钴、镍、锌、镓、硒、铷、锶、钡和铀是微量元素的主成分,可作为特征元素;26批白石脂样品可聚为4类。结论:该方法操作简便、分析快速、灵敏度高,能提高测定结果的精密度和准确性,适用于白石脂中重金属及微量元素的测定。

OBJECTIVE:To establish a method for simultaneous determination of 27 kinds of heavy metals and trace elements in Halloysitum album from different origins.METHODS:The sample was dissolved by wet digestion.Using inductively coupled plasma mass spectrometry(ICP-MS),carrier gas was argon and collision gas was helium;plasma gas flow rate was 15.0 L/min;flow rate of carrier gas was 1.17 L/min and collision gas flow rate was 5.0 mL/min;atomizer was Barbinton,and sampling depth was 8.0 mm;atomizing chamber temperature was 2℃;radio frequency power was 1.3 kW;peristaltic pump revolutions was 30 r/min.In full quantitative analysis model,the number of test points was 3,the analysis time was 0.1 s,the repetition was 3 times,clustering analysis was conducted by using PASW Statistics 18.0 software.RESULTS:The linear range of 27 kinds of heavy metals and trace elements were 0-200μg/L(r≥0.996 5);the quantitative limit was 0.003 41-75.485μg/L and the detection limit was 0.001 1-24.350 0μg/L.RSDs of precision,stability and repeatability tests were all less than 7%;average recovery was 72.3% -129.1% (RSD was 0.9% -9.4% ,n=6).The content of Al was 0.01-123 220.20 mg/kg,and Al was the element with the highest content.Li,Na,Mg,K,Ca,V,Mn,Fe,Co,Ni,Zn,Ga,Se,Rb,Sr,Ba and U were the principal components of trace elements and could be used as characteristic elements;26 batches of Halloysitum Album samples could be grouped into 4 categories.CONCLUSIONS:The established method is simple,fast and highly sensitive,can improve the precision and accuracy of test results,and it is suitable for the determination of heavy metals and trace elements in Halloysitum album.