Determination of urine melamine by validated isotopic ultra-performance liquid chromatography/tandem mass spectrometry

Wei Chih Cheng, Shu Kong Chen, Tien Jen Lin, I. Jen Wang, Ya Min Kao, Daniel Yang Chih Shin

Research output: Contribution to journalArticle

27 Citations (Scopus)

Abstract

Little is known about melamine (MEL) analysis in children's urine. In this study, an isotopic ultra-performance liquid chromatography/tandem mass spectrometry (UPLC/MS/MS) method was developed and systematically validated for the analysis of MEL in urine. The method is easily performed and comprises acidification, solid-phase extraction (SPE) and UPLC/MS/MS analysis. 13C3N3(1SNH2)3 was used as the internal standard (IS) for calibration. Transition ions m/z 127 > 85 of MEL and m/z 133 > 89 of the IS were used for quantification and m/z 127 > 68 of MEL was used for quantitative confirmation. Recovery and precision were assessed to guarantee the applicability of the method. The limit of quantification (LOQ) was 0.01 μg/mL while the calculated method detection limit was 0.006 μg/mL. The mean recoveries ranged from 96-99%. The method was then applied to analyze urine samples from children who had potentially consumed MEL-tainted dairy products during screening in Taiwan. Ten nephrolithiasis cases and 20 age- and gender-matched controls were selected for this study. Three out of the 10 nephrolithiasis cases had elevated levels of MEL. Comparatively, twenty age- and gender-matched non-nephrolithiasis controls consuming Taiwan brand milk powder all showed MEL levels lower than the detection limit except for two children with background levels of 0.02 μg/mL. The background level in these children urine samples was established by UPLC/MS/MS analysis. Positive results of urine MEL tests might be associated with nephrolithiasis in these candidates. Measurement of urine MEL concentration can be helpful in confirming MEL-related nephrolithiasis, but its clinical application needs further clarification.

Original languageEnglish
Pages (from-to)1776-1782
Number of pages7
JournalRapid Communications in Mass Spectrometry
Volume23
Issue number12
DOIs
Publication statusPublished - Jun 30 2009
Externally publishedYes

Fingerprint

Liquid chromatography
Mass spectrometry
melamine
Dairy products
Recovery
Acidification
Powders
Screening
Calibration
Ions

ASJC Scopus subject areas

  • Spectroscopy
  • Analytical Chemistry
  • Organic Chemistry

Cite this

Determination of urine melamine by validated isotopic ultra-performance liquid chromatography/tandem mass spectrometry. / Cheng, Wei Chih; Chen, Shu Kong; Lin, Tien Jen; Wang, I. Jen; Kao, Ya Min; Shin, Daniel Yang Chih.

In: Rapid Communications in Mass Spectrometry, Vol. 23, No. 12, 30.06.2009, p. 1776-1782.

Research output: Contribution to journalArticle

Cheng, Wei Chih ; Chen, Shu Kong ; Lin, Tien Jen ; Wang, I. Jen ; Kao, Ya Min ; Shin, Daniel Yang Chih. / Determination of urine melamine by validated isotopic ultra-performance liquid chromatography/tandem mass spectrometry. In: Rapid Communications in Mass Spectrometry. 2009 ; Vol. 23, No. 12. pp. 1776-1782.
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abstract = "Little is known about melamine (MEL) analysis in children's urine. In this study, an isotopic ultra-performance liquid chromatography/tandem mass spectrometry (UPLC/MS/MS) method was developed and systematically validated for the analysis of MEL in urine. The method is easily performed and comprises acidification, solid-phase extraction (SPE) and UPLC/MS/MS analysis. 13C3N3(1SNH2)3 was used as the internal standard (IS) for calibration. Transition ions m/z 127 > 85 of MEL and m/z 133 > 89 of the IS were used for quantification and m/z 127 > 68 of MEL was used for quantitative confirmation. Recovery and precision were assessed to guarantee the applicability of the method. The limit of quantification (LOQ) was 0.01 μg/mL while the calculated method detection limit was 0.006 μg/mL. The mean recoveries ranged from 96-99{\%}. The method was then applied to analyze urine samples from children who had potentially consumed MEL-tainted dairy products during screening in Taiwan. Ten nephrolithiasis cases and 20 age- and gender-matched controls were selected for this study. Three out of the 10 nephrolithiasis cases had elevated levels of MEL. Comparatively, twenty age- and gender-matched non-nephrolithiasis controls consuming Taiwan brand milk powder all showed MEL levels lower than the detection limit except for two children with background levels of 0.02 μg/mL. The background level in these children urine samples was established by UPLC/MS/MS analysis. Positive results of urine MEL tests might be associated with nephrolithiasis in these candidates. Measurement of urine MEL concentration can be helpful in confirming MEL-related nephrolithiasis, but its clinical application needs further clarification.",
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