微波消解-电感耦合等离子体质谱法测定文蛤中9种元素

Determination of 9 elements in clam by inductively coupled plasma mass spectrometry with microwave digestion

建立基于微波消解技术及电感耦合等离子体质谱法(ICP-MS)的文蛤样品中铬(^(52)Cr)、铁(^(57)Fe)、镍(^(60)Ni)、铜(^(63)Cu)、锌(^(66)Zn)、砷(^(75)As)、镉(^(111)Cd)、铊(^(205)Tl)、铅(^(208)Pb)的测定方法。以微波消解法处理样品,采用HNO_(3)作为消解用酸,并加入H_(2)O_(2)增强其消解能力。设定ICP-MS等离子体射频功率为1550 W,利用碰撞/反应池技术,以99.999%高纯氦气为碰撞气,流量为4.1 mL/min,采用动能歧视模式(KED)有效消除多原子分子产生的质谱干扰,以^(45)Sc、^(72)Ge、^(115)In、^(209)Bi作为内标元素,通过内标元素校正法有效降低基体干扰。9种元素的质量浓度在0.1~100.0μg/L范围内与目标元素荷质比信号强度线性关系良好,相关系数均大于0.999,方法检出限为0.001~0.150 mg/kg,样品加标回收率为83.4%~113.9%,测定结果的相对标准偏差为0.2%~3.4%(n=6)。所建立的方法简便高效,准确度好,灵敏度高,可满足文蛤中9种元素含量的测定要求。

A method for the determination of ^(52)Cr,^(57)Fe,^(60)Ni,^(63)Cu,^(66)Zn,^(75)As,^(111)Cd,^(205)Tl and ^(208)Pb in clam samples was established based on microwave digestion and inductively coupled plasma mass spectrometry(ICP-MS)technology.The samples were processed using microwave digestion with HNO_(3) as the digesting acid,augmented by the addition of H_(2)O_(2) to enhance its digesting capability.The ICP-MS plasma radiofrequency power was set at 1550 W,employing collision/reaction cell technology with 99.999%high-purity helium as the collision gas at a flow rate of 4.1 mL/min.The kinetic energy discrimination(KED)mode was used to effectively eliminate mass spectral interferences from polyatomic molecules.^(45)Sc,^(72)Ge,^(115)In,and ^(209)Bi were used as the internal standard elements to reduce matrix interferences through internal standard correction.The mass concentration of 9 elements had a good linear relationship with the charge to mass ratio intensity in the range of 0.1-100.0μg/L,with the correlation coefficients all more than 0.999,and the detection limits of the method was 0.001-0.150 mg/kg.The recoveries of sample spiking were 83.4%-113.9%,and the relative standard deviations of the determination results were 0.2%-3.4%(n=6).This method is characterized by its efficiency,high accuracy,and high sensitivity,meeting the requirements for the determination of the content of nine elements in actual clam samples.