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A novel mixed-mode solid phase extraction for simultaneous determination of melamine and cyanuric acid in food by hydrophilic interaction chromatography coupled to tandem mass chromatography.
J Chromatogr B Analyt Technol Biomed Life Sci. 2010 Oct 15; 878(28):2839-44.JC

Abstract

Utilizing a solid phase extraction column (MCT) containing mixed hydrophilic functional gel and cation exchange sorbent, a sensitive and rapid HPLC-MS/MS method for simultaneously determining the residues of melamine (MEL) and cyanuric acid (CYA) in human foodstuffs was developed. MEL and CYA in egg, pork, liver, kidney and pork, shrimp, sausage casing, honey, soybean milk, soybean powder and dairy product were extracted using acetonitrile/water, defatted with hexane and isolated using MCT solid phase extraction column. The residues were separated upon a hydrophilic interaction liquid chromatography (HILIC) column and analyzed by electrospray ionization under negative-positive switched mode on a triplequadrupole mass spectrometry. The selected reaction monitoring was performed on [M+H](+) of m/z 127.9 to provide the transition of 127>85 and 127>68 (MEL) while the [M-H](-) of m/z 127.1 was selected as the precursor ion for CYA resulting in product ions m/z 85 and 42. Isotope labeled internal standard ((15)N(3)-MEL and (13)C(3)-CYA) and matrix-matched calibration were both used to observe the recovery to be 70.0-129.6% and 70.0-128.9% with RSD of 1.4-23.3% and 1.5-21.7% for MEL and CYA, respectively (n=6). All the LODs and LOQs of MEL and CYA were less than 39.4 and 99.1μgkg(-1), respectively, in 18 matrices, which were sensitive enough for quantitative analysis. This method has been proven effective in simultaneous determination of melamine and cyanuric acid when inspecting unknown and positive samples.

Authors+Show Affiliations

Shanghai Entry-Exit Inspection and Quarantine Bureau of The People's Republic of China, Mingshen Rd 1208, Shanghai 200135, PR China. dengxj@shciq.gov.cnNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

20850393

Citation

Deng, Xiao-Jun, et al. "A Novel Mixed-mode Solid Phase Extraction for Simultaneous Determination of Melamine and Cyanuric Acid in Food By Hydrophilic Interaction Chromatography Coupled to Tandem Mass Chromatography." Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, vol. 878, no. 28, 2010, pp. 2839-44.
Deng XJ, Guo DH, Zhao SZ, et al. A novel mixed-mode solid phase extraction for simultaneous determination of melamine and cyanuric acid in food by hydrophilic interaction chromatography coupled to tandem mass chromatography. J Chromatogr B Analyt Technol Biomed Life Sci. 2010;878(28):2839-44.
Deng, X. J., Guo, D. H., Zhao, S. Z., Han, L., Sheng, Y. G., Yi, X. H., Zhou, Y., & Peng, T. (2010). A novel mixed-mode solid phase extraction for simultaneous determination of melamine and cyanuric acid in food by hydrophilic interaction chromatography coupled to tandem mass chromatography. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 878(28), 2839-44. https://doi.org/10.1016/j.jchromb.2010.08.038
Deng XJ, et al. A Novel Mixed-mode Solid Phase Extraction for Simultaneous Determination of Melamine and Cyanuric Acid in Food By Hydrophilic Interaction Chromatography Coupled to Tandem Mass Chromatography. J Chromatogr B Analyt Technol Biomed Life Sci. 2010 Oct 15;878(28):2839-44. PubMed PMID: 20850393.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - A novel mixed-mode solid phase extraction for simultaneous determination of melamine and cyanuric acid in food by hydrophilic interaction chromatography coupled to tandem mass chromatography. AU - Deng,Xiao-Jun, AU - Guo,De-Hua, AU - Zhao,Shan-Zhen, AU - Han,Li, AU - Sheng,Yong-Gang, AU - Yi,Xiong-Hai, AU - Zhou,Yao, AU - Peng,Tao, Y1 - 2010/09/17/ PY - 2010/07/11/received PY - 2010/08/23/revised PY - 2010/08/24/accepted PY - 2010/9/21/entrez PY - 2010/9/21/pubmed PY - 2011/1/25/medline SP - 2839 EP - 44 JF - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JO - J Chromatogr B Analyt Technol Biomed Life Sci VL - 878 IS - 28 N2 - Utilizing a solid phase extraction column (MCT) containing mixed hydrophilic functional gel and cation exchange sorbent, a sensitive and rapid HPLC-MS/MS method for simultaneously determining the residues of melamine (MEL) and cyanuric acid (CYA) in human foodstuffs was developed. MEL and CYA in egg, pork, liver, kidney and pork, shrimp, sausage casing, honey, soybean milk, soybean powder and dairy product were extracted using acetonitrile/water, defatted with hexane and isolated using MCT solid phase extraction column. The residues were separated upon a hydrophilic interaction liquid chromatography (HILIC) column and analyzed by electrospray ionization under negative-positive switched mode on a triplequadrupole mass spectrometry. The selected reaction monitoring was performed on [M+H](+) of m/z 127.9 to provide the transition of 127>85 and 127>68 (MEL) while the [M-H](-) of m/z 127.1 was selected as the precursor ion for CYA resulting in product ions m/z 85 and 42. Isotope labeled internal standard ((15)N(3)-MEL and (13)C(3)-CYA) and matrix-matched calibration were both used to observe the recovery to be 70.0-129.6% and 70.0-128.9% with RSD of 1.4-23.3% and 1.5-21.7% for MEL and CYA, respectively (n=6). All the LODs and LOQs of MEL and CYA were less than 39.4 and 99.1μgkg(-1), respectively, in 18 matrices, which were sensitive enough for quantitative analysis. This method has been proven effective in simultaneous determination of melamine and cyanuric acid when inspecting unknown and positive samples. SN - 1873-376X UR - https://www.unboundmedicine.com/medline/citation/20850393/A_novel_mixed_mode_solid_phase_extraction_for_simultaneous_determination_of_melamine_and_cyanuric_acid_in_food_by_hydrophilic_interaction_chromatography_coupled_to_tandem_mass_chromatography_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S1570-0232(10)00540-4 DB - PRIME DP - Unbound Medicine ER -