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- E-ISSN 2288-8985
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Uncertainty evaluation for the determination of creatinine in urine by LC-MS/MS
Analytical Science and Technology / Analytical Science and Technology, (P)1225-0163; (E)2288-8985
2012, v.25 no.1, pp.83-90
https://doi.org/10.5806/AST.2012.25.1.083
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(2012). Uncertainty evaluation for the determination of creatinine in urine by LC-MS/MS. Analytical Science and Technology, 25(1), 83-90, https://doi.org/10.5806/AST.2012.25.1.083
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Abstract
소변 중 크레아티닌의 정상적인 농도범위는 30 - 300 mg/dL로 마약류 감정에 앞서 크레아티닌농도를 측정함으로써 소변 시료의 유효성을 확인하고 있다. 크레아티닌 농도 측정을 위해 액체크로마토그래피-질량분량분석법(LC-MS/MS, liquid chromatography-tandem mass spectrometry)을 사용하였다. 우선소변 시료를 고속으로 원심분리한 후 10 μL를 분취하여 증류수 390 μL와 혼합하여 희석하였다. 희석된시료 20 μL에 내부표준물질(5 μg/mL) 30 μL와 acetonitrile 10 μL를 첨가하여 혼합한 후 여과한 시료를LC-MS/MS에 주입하였다. 크레아티닌은 multi-mode ODS column (Scherzo SM-C18, 75 × 2.0 mm, I.D. 3 μm)을 이용하여 분리하였고, 이동상은 0.2% formic acid와 acetonitrile로 구성되었으며 유속은 150 μL/min으로 하였다. 크레아티닌과 내부표준물질은 [M+H]+ precursor ion과 특징적인 product ion을 한 쌍으로 m/z 114.0→ 86.0과 m/z 117.0→ 89.1에서 모니터링하여 정량에 적합한 크로마토그램을 얻을 수 있었다. 측정불확도 평가에 앞서 정량분석시 측정값에 영향을 주는 인자들을 찾아내고 각각의 요소들이 측정결과에 어떤 영향을 주는가를 살펴보았다. 시료 희석, 검정 곡선, 재현성, 표준물질의 인자 순으로 측정불확도에 영향을 미치고 있음을 확인하였다. 실제 사람의 소변에서 크레아티닌 농도를 측정한 결과, 측정값에 대한 오차 범위의 상대불확도는 14.2%로 산출되었다.
- keywords
- Measurement uncertainty, urine analysis, creatinine, LC-MS/MS
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