ICP-MS法同时测定益中生血片中12种微量元素的含量

Simultaneous Determination of 12 Kinds of Microelements in Yizhong Shengxue Tablets by ICP-MS

目的:建立同时测定益中生血片中12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 350W,等离子体气流量为15.0 L/min,载气流量为1.12 L/min,氧化物指标(氧化铈离子/铈)<0.5%,双电荷指标(二价钡离子/一价钡离子)<1%,积分时间为0.1 s,雾化器为高盐雾化器,雾化室温度为2℃,重复次数为3次,蠕动泵转速分辨率为0.1 rps,采样深度为7.0 mm,微波消解功率为3 600 W,升温程序为190℃保持48 h,冷却至室温,再升温至150℃,保持12 h。结果:硼、钒、铬、锰、钴、镍、铜、锌、硒、铷、钼、锡元素检测质量浓度线性范围分别为0.05～150μg/L(r=0.999 8)、0.05～150μg/L(r=0.999 7)、0.05～150μg/L(r=0.999 5)、0.05～150μg/L(r=0.999 6)、0.05～150μg/L(r=0.999 7)、0.05～150μg/L(r=0.999 8)、0.05～150μg/L(r=0.999 6)、0.05～150μg/L(r=0.999 8)、0.05～150μg/L(r=0.999 5)、0.05～150μg/L(r=0.999 9)、0.05～150μg/L(r=0.999 6)、0.05～150μg/L(r=0.999 7);定量限分别为0.017、0.007、0.021、0.042、0.013、0.017、0.018、0.019、0.020、0.011、0.011、0.018μg/L,检测限分别为0.005、0.002、0.007、0.011、0.003、0.005、0.004、0.004、0.006、0.003、0.003、0.005μg/L;精密度、稳定性、重复性试验的RSD均小于6%;加样回收率为95.138%～104.928%(RSD为0.96%～2.97%,n=9);平均含量分别为5.266、0.453、1.581、170.600、11.280、5.204、1.560、24.300、0.987、7.302、0.239、0.702μg/g。结论:该方法快速、灵敏度高、准确度好,可用于同时测定益中生血片中12种微量元素的含量;益中生血片样品中Mn、Zn、Co、Rb、B元素的含量相对较高。

OBJECTIVE:To establish a method for simultaneous determination of 12 kinds of microelements in Yizhong shengxue tablets.METHODS:ICP-MS method was adopted.Rf power was set at 1 350 W;plasma gas velocity was 15.0 L/min and carrier gas velocity was 1.12 L/min;the oxide index(CeO+/Ce)was less than 0.5%,and the double charge index(Ba2+/Ba+)was less than 1%;the integration time was 0.1 s,high salt atomizer was used,which atomizing chamber temperature was 2℃;repetition times was 3 times;the peristaltic pump frequency was 0.1 rps and the sampling depth was 7.0 mm.The microware digestion power was 3 600 W and the heating process was heated to 190℃maintaining for 48 h,and then cooled to room temperature,finally heated to 150℃maintaining for 12 h.RESULTS:The linear range of B,V,Cr,Mn,Co,Ni,Cu,Zn,Se,Rb,Mo and Sn were 0.05-150μg/L(r=0.999 8),0.05-150μg/L(r=0.999 7),0.05-150μg/L(r=0.999 5),0.05-150μg/L(r=0.999 6),0.05-150μg/L(r=0.999 7),0.05-150μg/L(r=0.999 8),0.05-150μg/L(r=0.999 6),0.05-150μg/L(r=0.999 8),0.05-150μg/L(r=0.999 5),0.05-150μg/L(r=0.999 9),0.05-150μg/L(r=0.999 6),0.05-150μg/L(r=0.999 7),respectively.The limits of quantitation were 0.017,0.007,0.021,0.042,0.013,0.017,0.018,0.019,0.020,0.011,0.011,0.018μg/L;the limits of detection were 0.005,0.002,0.007,0.011,0.003,0.005,0.004,0.004,0.006,0.003,0.003,0.005μg/L,respectively.RSDs of precision,stability and reproducibility tests were all lower than 6%.The recoveries were 95.138%-104.928%(RSDs were 0.96%-2.97%,n=9).Average contents of 12 kinds of microelements were 5.266,0.453,1.581,170.600,11.280,5.204,1.560,24.300,0.987,7.302,0.239 and 0.702μg/g.CONCLUSIONS:Established method is rapid,sensitive and accurate for simultaneous determination of 12 kinds of microelements in Yizhong shengxue tablets.The contents of Mn,Zn,Co,Rb and B in Yizhong shengxue tablets were relatively high.