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流动注射-电感耦合等离子体质谱法测定尿液中铀和钍同位素

Flow-injection technique for determination of uranium and thorium isotopes in urine by inductively coupled plasma mass spectrometry.

作者信息

Benkhedda Karima, Epov Vladimir N, Evans R Douglas

机构信息

Environmental Resources Studies, Trent University, 1600 West Bank Drive, Peterborough, Ontario, K9J 7B8, Canada.

出版信息

Anal Bioanal Chem. 2005 Apr;381(8):1596-603. doi: 10.1007/s00216-005-3147-y. Epub 2005 Apr 13.

Abstract

A sensitive and efficient flow-injection (FI) preconcentration and matrix-separation technique coupled to sector field ICP-mass spectrometry (SF-ICP-MS) has been developed and validated for simultaneous determination of ultra-low levels of uranium (U) and thorium (Th) in human urine. The method is based on selective retention of U and Th from a urine matrix, after microwave digestion, on an extraction chromatographic TRU resin, as an alternative to U/TEVA resin, and their subsequent elution with ammonium oxalate. Using a 10 mL sample, the limits of detection achieved for 238U and 232Th were 0.02 and 0.03 ng L(-1), respectively. The accuracy of the method was checked by spike-recovery measurements. Levels of U and Th in human urine were found to be in the ranges 1.86-5.50 and 0.176-2.35 ng L(-1), respectively, well in agreement with levels considered normal for non-occupationally exposed persons. The precision obtained for five replicate measurements of a urine sample was 2 and 3% for U and Th, respectively. The method also enables on-line measurements of the 235U/238U isotope ratios in urine. Precision of 0.82-1.04% (RSD) was obtained for 235U/238U at low ng L(-1) levels, using the FI transient signal approach.

摘要

一种灵敏且高效的流动注射(FI)预浓缩和基体分离技术与扇形场电感耦合等离子体质谱(SF-ICP-MS)联用,已被开发并验证用于同时测定人尿中超低水平的铀(U)和钍(Th)。该方法基于在微波消解后,将尿液基体中的U和Th选择性保留在萃取色谱TRU树脂上(作为U/TEVA树脂的替代物),然后用草酸铵进行洗脱。使用10 mL样品时,238U和232Th的检测限分别为0.02和0.03 ng L(-1)。通过加标回收测量来检验该方法的准确性。发现人尿中U和Th的含量分别在1.86 - 5.50和0.176 - 2.35 ng L(-1)范围内,与非职业暴露人群的正常水平相符。对一份尿样进行五次重复测量得到的精密度,U和Th分别为2%和3%。该方法还能够在线测量尿中235U/238U同位素比值。使用FI瞬态信号方法,在低ng L(-1)水平下,235U/238U的精密度为0.82 - 1.04%(相对标准偏差)。

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