Dissertation > Environmental science, safety science > Environmental Quality Assessment and Environmental Monitoring > Environmental monitoring > General issues > Monitoring and analysis methods

Method Research for Simultaneous Determination of Melamine, Cyanuric Acid and Uric Acid by Reversed Phase High Performance Liquid Chromatography

Author LiYuYu
Tutor HanHongLin
School Beijing Jiaotong University
Course Environmental Engineering
Keywords High Performance Liquid Chromatography C18 Melamine Cyanuric acid Uric acid
CLC X830.2
Type Master's thesis
Year 2010
Downloads 205
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- RP-HPLC method for simultaneous detection of melamine, cyanuric acid, uric acid C18 column There is no study for the establishment of the method of in-depth discussions. Of each ion on the buffer solution, phosphate buffer solution as the mobile phase, to discuss the pH, the proportion of the mobile phase, detection wavelength was analyzed on a C18 column of melamine, cyanuric acid, uric acid, and eventually the initial establishment of a simultaneous detection of these three substances The reversed-phase high performance liquid chromatography. The analysis method is applied to the plasma, stone samples, the results showed that the sample matrix interference of the analytes is not serious, basically meet the analytical requirements. Pass the test precision, limit of detection, limit of quantification, the recovery of the analysis of reliability of the method has been verified. The contents and conclusions are as follows: (1) the liquid phase selection and optimization of the conditions under the premise of the organic phase, ion of the buffer solution and phosphate buffer solution as the water phase system, optimizing the proportion of mobile phase: acetonitrile as detection wavelength, the pH of the mobile phase C18 column separation of melamine, cyanuric acid, uric acid. The results show that the buffer solution as the mobile phase ion cyanuric acid can not be detected, only the simultaneous analysis of melamine and uric acid. Mobile phase 90% ion buffer solution (octane-sodium citrate, pH = 3.0) 10% acetonitrile, detection wavelength 280nm 4.5min switch for 240nm, under this condition, the melamine and uric acid can be obtained very good separation; mobile phase was 100% phosphate buffer solution (10 mmol / L, pH = 7.50), the detection wavelength was 200nm, under these conditions, C18 column can be a good separation of melamine, cyanuric acid and uric acid; (2) application and verification of the analytical methods: ① the selection and optimization of sample pre-treatment: identify a set of pre-treatment program tenet of simple, low-cost extraction solvent acetonitrile aqueous solution. 2:1 aqueous acetonitrile as the extracting solvent, is not only able to precipitate protein and do not waste acetonitrile results showed that the treatment effect of different proportions (1:1,2:1,3:1) aqueous acetonitrile. Measured by the actual sample target matrix interference is not serious, that the pre-treatment methods (ultrasonic extraction, centrifugation, dried with nitrogen, the reconstitution of pure water) to meet the analytical requirements. ② Validation of Analytical Procedures: unknown sample of a plasma measured repeated 6 times, the calculation of retention time and peak area relative standard deviation, and results show that the method is a high precision within the range of 0.48% to 1.00%; to the signal-to-noise ratio of 3 to determine minimum detection limit of melamine, cyanuric acid, uric acid were: 0.0045μg/mL. 0.0248μg/mL 0.0231μg/mL signal-to-noise ratio of 10 to determine melamine, cyanuric acid, uric acid The lower limit of quantification were: 0.015μg/mL 0.083μg/mL 0.078μg/mL results show that this method has high sensitivity; spiked recovery test set 5μg/mL, 10μg/mL two concentrations of The recoveries of the three substances are within the range of 92.59% to 107.26%, indicating a very high accuracy of the method.

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