Quarles C Derrick, Jones Deanna R, Jarrett Jeffery M, Shakirova Gulchekhra, Pan Yi, Caldwell Kathleen L, Jones Robert L
Inorganic & Radiation Analytical Toxicology Branch, National Center for Environmental Health, Centers for Disease Control and Prevention, 4770 Buford Highway, Mailstop F-18, Atlanta, GA 30341.
J Anal At Spectrom. 2014;2014(2):297-303. doi: 10.1039/C3JA50272D.
Biomonitoring and emergency response measurements are an important aspect of the Division of Laboratory Sciences of the National Center for Environmental Health, Centers for Disease Control and Prevention (CDC). The continuing advancement in instrumentation allows for enhancements to existing analytical methods. Prior to this work, chromium and nickel were analyzed on a sector field inductively coupled plasma-mass spectrometer (SF-ICP-MS). This type of instrumentation provides the necessary sensitivity, selectivity, accuracy, and precision but due to the higher complexity of instrumentation and operation, it is not preferred for routine high throughput biomonitoring needs. Instead a quadrupole based method has been developed on a PerkinElmer NexION 300D ICP-MS. The instrument is operated using 6.0 mL min helium as the collision cell gas and in kinetic energy discrimination mode, interferences are successfully removed for the analysis of Cr (ArC and ClOH) and Ni (CaO). The limits of detection are 0.162 μg L Cr and 0.248 μg L Ni. Method accuracy using NIST SRM 2668 level 1 (1.08 μg L Cr and 2.31μg L Ni) and level 2 (27.7 μg L Cr and 115 μg L Ni) was within the 95% confidence intervals reported in the NIST certificate. Among-run precision is less than 10% RSDs (N = 20) for in house quality control and NIST SRM urine samples. While the limits of detection (LOD) for the new quadrupole ICP-UCT-MS with KED method are similar to the SF-ICP-MS method, better measurement precision is observed for the quadrupole method. The new method presented provides fast, accurate, and more precise results on a less complex and more robust ICP-MS platform.
生物监测和应急响应测量是美国疾病控制与预防中心(CDC)国家环境卫生中心实验室科学部的一个重要方面。仪器的不断进步使得现有分析方法得以改进。在这项工作之前,铬和镍是在扇形场电感耦合等离子体质谱仪(SF-ICP-MS)上进行分析的。这种类型的仪器提供了必要的灵敏度、选择性、准确性和精密度,但由于仪器和操作的复杂性较高,它不太适合常规高通量生物监测需求。相反,已在珀金埃尔默NexION 300D ICP-MS上开发了一种基于四极杆的方法。该仪器使用6.0 mL/min的氦气作为碰撞池气体进行操作,并在动能歧视模式下,成功消除了Cr(ArC和ClOH)和Ni(CaO)分析中的干扰。检测限分别为0.162 μg/L Cr和0.248 μg/L Ni。使用NIST SRM 2668一级(1.08 μg/L Cr和2.31 μg/L Ni)和二级(27.7 μg/L Cr和115 μg/L Ni)的方法准确度在NIST证书报告的95%置信区间内。对于内部质量控制和NIST SRM尿液样本,批间精密度小于10% RSD(N = 20)。虽然采用KED方法的新型四极杆ICP-UCT-MS的检测限与SF-ICP-MS方法相似,但四极杆方法的测量精密度更高。本文提出的新方法在一个不太复杂且更稳健的ICP-MS平台上提供了快速、准确和更精确的结果。