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LC-MS quantitative detection method for melamine and tricyanic acid in human urine

A technology of melamine and cyanuric acid, which is applied in the field of medical testing, can solve the problems that the detection methods of melamine and cyanuric acid have not been reported yet, and achieve the effect of simple operation, high sensitivity and strong specificity

Inactive Publication Date: 2012-01-04
CENT HOSPITAL XUHUI DISTRICT SHANGHAI CITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] There is no report about the detection method of melamine and cyanuric acid in human urine

Method used

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  • LC-MS quantitative detection method for melamine and tricyanic acid in human urine
  • LC-MS quantitative detection method for melamine and tricyanic acid in human urine
  • LC-MS quantitative detection method for melamine and tricyanic acid in human urine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Detection conditions and method examples

[0037] 1. Reagent preparation:

[0038] (1) Standard curve: absorb appropriate amount of standard working solution of melamine and cyanuric acid, add double distilled water, and make respectively 10, 50, 100, 500, 1000, 2500, 5000ng / ml containing melamine and cyanuric acid standard aqueous solution. Contains 7 concentration points, each concentration is prepared with 1ml.

[0039] (2) Quality control product: absorb appropriate amount of standard working solution of melamine and cyanuric acid, add double distilled water, and make melamine and cyanuric acid containing melamine and cyanuric acid with concentration of 10, 20, 2000, 4000ng / ml respectively Acid is used as a quality control product, containing 4 concentration points, and 2ml is prepared for each concentration.

[0040] (3) Internal standard: draw 250 μl melamine internal standard (100 μg / ml) solution into a 10ml volumetric flask, dilute to volume with 50% methanol...

Embodiment 2

[0096] Chromatographic conditions

[0097] Reagent preparation, sample collection and sample processing methods and detection conditions are the same as in Example 1. In chromatographic conditions, use Thermo Hypersil Silica (150mm × 2.1mm i.d., 5 μm, Thermo) analysis column for melamine instead, isocratic elution, mobile phase (A) 0.0001% formic acid water, (B) 0.0001% formic acid acetonitrile, A: B is The volume ratio is 15:85. Under these conditions, the retention time of melamine and internal standard is 2.6min. Cyanuric acid adopts RESTEK Allure PFP Propyl (100mm×2.1mm i.d., 5μm, RESTEK) analytical column, isocratic elution, mobile phase (A) 0.1% formic acid water, (B) 0.1% formic acid 50% acetonitrile 50% methanol , A: B is a volume ratio of 30:70. Under these conditions, the retention time of cyanuric acid and internal standard is 1.3min. The chromatographic peak shapes of melamine and cyanuric acid are good, and there is no interference at the corresponding chromat...

Embodiment 3

[0099] Methodology Validation

[0100] Using the detection conditions and methods listed in Example 1, the assay method was validated methodologically. In the concentration range of 10-5000ng / ml melamine and cyanuric acid, the linear relationship is good (r≥0.9990), and the lowest detection limit can reach 1ng / ml. The intra-assay and inter-assay precision RSDs were ≤3.26% and ≤5.43%, respectively, and the accuracy was 93.7-102.8%. The extraction recovery rate was 78.0-83.3%, the RSD≤4.6%, and the medium effect was 96.4-97.6%. The results of the method validation show that LC-MS / MS can detect a large number of clinical samples sensitively, accurately and rapidly.

[0101] 1. Standard curve and quantitative range

[0102] A standard curve was prepared according to the method in Example 1, and three batches of processing and sample injection were carried out to obtain 3 sets of standard curves. Taking the concentration as the x-axis, and the ratio of the peak areas of melamin...

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Abstract

The invention discloses an LC-MS quantitative detection method for melamine and tricyanic acid in human urine. The method is characterized in that the isotope dilution technology is adopted, and in pre-processing of an urine sample, 13C3, 15N3-melamine or deuterated melamine, 13C3 and 15N3-tricyanic acid are respectively added in interior label solution; melamine and tricyanic acid in human urineare respectively extracted by a liquid-liquid extraction method; an LC-MS / MS method is established to respectively and quantitatively detect the concentration of melamine and tricyanic acid in human urine; a liquid chromatogram takes filled columns such as phenyl, fluorophenyl, silica gel and the like as immobile phase; methanol, acetonitrile, water, formic acid solution or mixed liquid as mobilephase; in chromatographic resolution, isocratic elution or gradient elution is carried out; and in mass spectrometric detection, an ESI Source is used for detecting the content of melamine and tricyanic acid in human urine. The minimum limit of quantification of melamine and tricyanic acid can reach 10ng / ml. The processing of a sample by the method in the invention is economical, simple and convenient, in addition, the detection has strong specificity and high sensitivity, and various methodology indicators can reach related technological requirements of the Chinese Pharmacopoeia.

Description

technical field [0001] The invention relates to the technical field of medical detection, in particular to a quantitative detection method for melamine and cyanuric acid in human urine. Background technique [0002] Melamine (Melamine, 2,4,6-triamino-1,3,5-triazine) is a triazine nitrogen-containing heterocyclic organic compound with molecular formula C 3 N 3 (NH 2 ) 3 , molecular weight 126.12. The structural formula is: [0003] [0004] When melamine is hydrolyzed with strong acid or strong alkali aqueous solution, the amine group is gradually replaced by hydroxyl group, first to generate ammeline, further hydrolyzed to generate ammeline, and finally to generate cyanuric acid: [0005] [0006] Since protein is mainly composed of amino acids, its nitrogen content is generally no more than 30%, and the molecular formula of melamine (C 3 N 6 h 6 ) nitrogen content is 66.7%. At this stage, the general protein testing method "Kjeldahl method" is to estimate the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/26
Inventor 朱建民余琛何健刘罡一高淳新陆川张梦琪李水军戴方刘昀周菊珍宋晓涛贾晶莹刘艳梅周红
Owner CENT HOSPITAL XUHUI DISTRICT SHANGHAI CITY
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