Determination of Residual Cyromazine and Its Metabolite Melamine in Pig Urine Samples Using Ultrahigh Performance Liquid Chromatography Coupled with Quadrupole-Orbitrap Mass Spectrometry
Experimental Techniques and Methods|更新时间:2023-02-13
|
Determination of Residual Cyromazine and Its Metabolite Melamine in Pig Urine Samples Using Ultrahigh Performance Liquid Chromatography Coupled with Quadrupole-Orbitrap Mass Spectrometry
Journal of Instrumental AnalysisVol. 40, Issue 12, Pages: 1784-1789(2021)
LUO Qiu-hong,HAN Ying,HU Bei,et al.Determination of Residual Cyromazine and Its Metabolite Melamine in Pig Urine Samples Using Ultrahigh Performance Liquid Chromatography Coupled with Quadrupole-Orbitrap Mass Spectrometry[J].Journal of Instrumental Analysis,2021,40(12):1784-1789.
LUO Qiu-hong,HAN Ying,HU Bei,et al.Determination of Residual Cyromazine and Its Metabolite Melamine in Pig Urine Samples Using Ultrahigh Performance Liquid Chromatography Coupled with Quadrupole-Orbitrap Mass Spectrometry[J].Journal of Instrumental Analysis,2021,40(12):1784-1789. DOI: 10.19969/j.fxcsxb.21032306.
Determination of Residual Cyromazine and Its Metabolite Melamine in Pig Urine Samples Using Ultrahigh Performance Liquid Chromatography Coupled with Quadrupole-Orbitrap Mass Spectrometry
An ultrahigh performance liquid chromatography coupled with quadrupole-orbitrap mass spectrometry(UHPLC-Quadrupole-Orbitrap MS) was developed for the determination of cyromazine and its metabolite melamine in pig urine samples.The pig urine sample(2.0 g) was ultrasonically extracted with 1% trichloroacetic acid under the pH value of the extraction mixture lower than 3,followed by purification with a mixed cation solid phase extraction column(MCX),then the eluent from the MCX column was blow dried under nitrogen flow,and finally reconstituted with 95% acetonitrile aqueous solution.The reconstituted solution 10 times diluted was injected into the UHPLC-Quadrupole-Orbitrap system using a Syncronis HILIC column(100 mm × 2.1 mm,1.7 μm) at 35 ℃,with 10 mmol/L ammonium acetate and acetonitrile as the mobile phases.The mass spectrometer was operated in positive electrospray(ESI + ) and parallel reaction monitoring(PRM) mode.Qualitative analysis was carried out according to the accurate masses of each target compound,its fragment ions,and the abundance ratios of the fragment ions.The external standard method and internal standard method were used for the quantification of cyromazine and melamine,respectively.Method validation showed that there were good linear relationships for the two targets in the range of 0.2-50.0 ng/mL,with their correlation coefficients(,r,2,) larger than 0.99.At three spiked levels of 1.0,2.0 and 150.0 μg/kg,the recoveries for cyromazine and melamine in pig urine sample ranged from 78.0% to 105%,with relative standard deviations(RSD) no more than 11%.The same spiked samples were used for comparison between PRM of orbitrap and multiple reaction monitoring(MRM) mode of triple quadrupole.The results obtained exhibited no significant difference,indicating that both methods have good quantitative ability for determination of cyromazine and melamine in pig urine sample.With good recovery,dynamic range and quantification accuracy,the developed method could be applied to the simultaneous qualitative and quantitative analyses of cyromazine and melamine residues in pig urine samples.
关键词
猪尿环丙氨嗪三聚氰胺超高效液相色谱-四极杆/静电场轨道阱质谱
Keywords
pig urinecyromazinemelamineultrahigh performance liquid chromatography coupled with quadrupole-orbitrap mass spectrometry
references
Taylor D B,Friesen K,Zhu J J,Sievert K.J. Econ. Entomol.,2012,105(2):726-731.
Chen Q,Pan X D,Huang B F,Han J L.J. Pharm. Biomed. Anal.,2017,145(25):525-530.
2002/657/EC Implementing Council Directive 96/23/EC Concerning the Performance of Analytical Methods and the Interpretation of Results.
GB 29704-2013.National Food Safety Standards.Determination of Cyromazine and Its Metabolite Melamine in Animal Food by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry.National Standards of the People’s Republic of China(食品安全国家标准 动物性食品中环丙氨嗪及代谢物三聚氰胺多残留的测定 超高效液相色谱-串联质谱法.中华人民共和国国家标准).
Shi X Y.Sci. Technol. Rev. (史雪岩.科技导报),2010,28(4):101-109.
Zhou X Q,Lü X L,Wan J C,Guo P,Guo D,Xi H T.Chin. J. Chromatogr. (周晓倩,吕小丽,万建春,郭平,郭丹,席慧婷.色谱),2019,37(10):1064-1070.
GB/T 27404-2008.Criterion on Quality Control of Laboratories-Chemical Testing of Food.National Standards of the People’s Republic of China(实验室质量控制规范 食品理化检测.中华人民共和国国家标准).
Determination of Melamine Migration in Melamine Tableware by LC-ESI MS/MS
Determination of Clenbuterol and Chloramphenicol in Pig Urine Using Dispersive Liquid-Liquid Microextraction with High Performance Liquid Chromatography-Tandem Mass Spectrometry
Sensitive Determination of Melamine by Field Enhanced Sample Injection-Capillary Zone Electrophoresis Technique
Rapid Determination of Melamine in Milk Power and Milk Based on Jet Type Electrochemiluminescence Flow System
Performance Study of a New Reversed-phase and Strong Cationic Exchange Solid Phase Extraction Cartridge