title: [Simultaneous determination of melamine and cyanuric acid residues in water and urine by solid phase extraction-hydrophilic interaction liquid chromatography-electrospray tandem mass spectrometry method].
abstract: OBJECTIVE
  We aimed to establish a sensitive quantified method for the simultaneous determination of melamine and cyanuric acid residues in water and urine by hydrophilic interaction liquid chromatography coupled with electrospray tandem mass spectrometry (HILIC-ESI-MS/MS) with the pretreatment of hydrophilic functional silica gel and cation exchange resin mixed solid phase extraction column(MCT), and to investigate the melamine and cyanuric acid residues in 501 water and 216 urine from several province and city.
  
  
  METHODS
  About 100 ml water (or 10 ml urine) was adjusted to pH 3.0 with concentrated hydrochloric acid, and then mixed with the internal standard solution((15)N3-melamine and (15)N3-(13)C3 -cyanuric acid) and 100 ml acetonitrile (10 ml for urine). The solution was cleaned with MCT solid-phase extraction column, and eluted once by 3 ml methanol and twice by 2.5 ml methanol (containing 5% ammonia water). The effluent was collected and dried by N2 flow at 40 °C, and then diluted to 2 mmol/L ammonium acetate containing 90% volume fraction acetonitrile. The completely dissolved solution was then filtered with 0.22 µm organic membrane; and the filtrate was detected by high performance liquid chromatography-tandem mass spectrometry and quantified with internal standards. The repeatability and sensitivity of the assay were evaluated. Then we detected the melamine and cyanuric acid residues in 501 water and 216 urine samples collected from several province and city.
  
  
  RESULTS
  By the quantification of internal standard (15)N3-melamine and (15)N3-(13)C3-cyanuric acid, the melamine and cyanuric acid were linear in the range of 2.0-1000.0 µg/L with correlation coefficient of 0.9998 and 0.9997. The detection limits of the method were separately 0.4 ng/L (melamine) and 0.3 ng/L (cyanuric acid) for water, and 4.0 ng/L (melamine) and 3.0 ng/L (cyanuric acid) for urine. The average recovery rate was around 95.3%-100.1% with the relative standard deviation (RSD) was <4.02%. Out of the 501 water samples, melamine was detected out in 19.9% (100/501) and cyanuric acid was detected out in 5.2% (26/501). The content was around 0.03-5.00 g/L. Melamine or cyanuric acid was detected out in 24.5% of the urine samples (53/216), with the content around 0.01-1.00 g/L.
  
  
  CONCLUSIONS
  The established method of solid phase extraction-hydrophilic interaction liquid chromatography-electrospray tandem mass spectrometry can satisfy the requirement for detection of melamine and cyanuric acid residues in all sorts of water and urine. Meanwhile, the two substances widely existed in water and Chinese population.
authors.affiliation: Physical and Chemical Testing Division, Shenzhen Center for Disease Control and Prevention, Shenzhen 518055, China. Email: liuhonghe@sina.com.
authors.forename: Hong-he
authors.initials: HH
authors.lastname: Liu
authors.forename: Li-sha
authors.initials: LS
authors.lastname: Mao
authors.forename: Li
authors.initials: L
authors.lastname: Kang
authors.forename: Gui-hua
authors.initials: GH
authors.lastname: Liu
authors.forename: Chao-qiong
authors.initials: CQ
authors.lastname: Peng
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods; D004784:Environmental Monitoring / Q000379:methods*; D006801:Humans; D013058:Mass Spectrometry; D052616:Solid Phase Extraction / Q000379:methods; D014227:Triazines / Q000032:analysis* / Q000652:urine; D016482:Urinalysis / Q000379:methods*
chemical_list: D014227:Triazines; C004632:cyanuric acid; C011907:melamine