PMID- 23845887 OWN - NLM STAT- MEDLINE DCOM- 20150421 LR - 20140709 IS - 1945-239X (Electronic) IS - 0021-9665 (Linking) VI - 52 IP - 7 DP - 2014 Aug TI - A sensitive and validated HPLC method for the determination of cyromazine and melamine in herbal and edible plants using accelerated solvent extraction and cleanup with SPE. PG - 751-7 LID - 10.1093/chromsci/bmt089 [doi] AB - A highly sensitive method was developed for the determination of the residues of cyromazine (CYR) and its metabolite, melamine (MEL), in herbal and edible plant samples by using reversed phase high-performance liquid chromatography-diode-array detection (RP-HPLC-DAD) with accelerated solvent extraction and solid phase extraction cleanup. The conditions of separation and detection were investigated and optimized. A Waters C18 column (250 x 4.6 mm i.d., 5 microm) was used for the RP-HPLC, with a mobile phase composed of 0.1% trifluoroacetic acid solution and methanol (85:15, v/v, pH 2.6). Under the optimized conditions, good linearity was achieved with a correlation coefficient of 0.9998. The limits of quantification of the method were 2.15 microg/kg for CYR and 2.51 microg/kg for MEL, which are maximum residue limits as low as three orders of magnitude. The recovery values at three spiked concentrations were in the range of 96.2-107.1% with relative standard deviations (RSDs) of 1.1-5.7% for CYR, and 92.7-104.9% with RSDs of 1.7-6.1% for MEL. The proposed method allows detection at levels as low as microg/kg levels for CYR and MEL. The method was validated by liquid chromatography-tandem mass spectrometry, and can be used for the routine determination of CYR and MEL in herbal and edible plant samples with the characteristics of speed, high sensitivity and accuracy, and low consumption of reagents. CI - (c) The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com. FAU - Ge, Xusheng AU - Ge X AD - College of Chemistry and Environmental Science, Hebei University, Key Laboratory of Analytical Science and Technology of Hebei Province, Wusi East Road 180, Baoding, 071002, P. R. China Biochemical Department, Baoding University, Qiyi East Road 3027, Baoding, 07100, P. R. China. FAU - Wu, Xingqiang AU - Wu X AD - College of Chemistry and Environmental Science, Hebei University, Key Laboratory of Analytical Science and Technology of Hebei Province, Wusi East Road 180, Baoding, 071002, P. R. China. FAU - Liang, Shuxuan AU - Liang S AD - College of Chemistry and Environmental Science, Hebei University, Key Laboratory of Analytical Science and Technology of Hebei Province, Wusi East Road 180, Baoding, 071002, P. R. China. FAU - Sun, Hanwen AU - Sun H AD - College of Chemistry and Environmental Science, Hebei University, Key Laboratory of Analytical Science and Technology of Hebei Province, Wusi East Road 180, Baoding, 071002, P. R. China gexusheng@163.com. LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20130711 PL - United States TA - J Chromatogr Sci JT - Journal of chromatographic science JID - 0173225 RN - 0 (Triazines) RN - CA49Y29RA9 (cyromazine) RN - N3GP2YSD88 (melamine) SB - IM MH - Chromatography, High Pressure Liquid/*methods MH - Least-Squares Analysis MH - Plants, Edible/*chemistry MH - Plants, Medicinal/*chemistry MH - Reproducibility of Results MH - Sensitivity and Specificity MH - Solid Phase Extraction/*methods MH - Triazines/*analysis EDAT- 2013/07/13 06:00 MHDA- 2015/04/22 06:00 CRDT- 2013/07/13 06:00 PHST- 2013/07/13 06:00 [entrez] PHST- 2013/07/13 06:00 [pubmed] PHST- 2015/04/22 06:00 [medline] AID - bmt089 [pii] AID - 10.1093/chromsci/bmt089 [doi] PST - ppublish SO - J Chromatogr Sci. 2014 Aug;52(7):751-7. doi: 10.1093/chromsci/bmt089. Epub 2013 Jul 11.