PMID- 25185313 OWN - NLM STAT- MEDLINE DCOM- 20150901 LR - 20190923 IS - 1000-8713 (Print) IS - 1000-8713 (Linking) VI - 32 IP - 5 DP - 2014 May TI - [Determination of cefalonium residue in milk by high performance liquid chromatography-tandem mass spectrometry]. PG - 519-23 AB - An analytical method was developed for the determination of cefalonium in milk by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). A total of 1 g milk was deproteinized by acetonitrile. The supernatant was transferred into a test tube to be blown dry with N2 at 37 degrees C. Then the residue was dissolved with methanol-0.1% formic acid in water (3:7, v/v). The sample was determined by HPLC-MS/MS after the purification. The chromatographic separation was achieved on a C18 column using 0.1% formic acid in water and acetonitrile as mobile phases with gradient elution. Qualitative and quantitative analyses were achieved by HPLC-MS/MS under positive ionization and multiple reaction monitoring (MRM) mode. Matrix-matched calibration curve was used for the quantification. Good correlation coefficients were obtained (r > 0. 999) in the mass concentration range of 2-200 microg/L. The limit of detection (LOD, S/N > or = 3) was 0.5 microg/kg in milk, and the limit of quantification (LOQ, S/N 10) was 2 microg/kg. The mean recoveries at the four levels of LOQ, 1/2MRL (maximum residue level), MRL, 2MRL were between 78.5% and 86.2%, with the intra-day relative standard deviations (RSDs) of 1.5% to 6.2% and inter-day RSDs of 2.9% to 5.6%. In conclusion, the established method can be applied for the determination of cefalonium residue in milk. FAU - Li, Shuaipeng AU - Li S FAU - Guo, Chunna AU - Guo C FAU - Meng, Lei AU - Meng L FAU - Huang, Xianhui AU - Huang X LA - chi PT - Journal Article PL - China TA - Se Pu JT - Se pu = Chinese journal of chromatography JID - 9424804 RN - 0 (Cephalosporins) SB - IM MH - Animals MH - Cephalosporins/*analysis MH - Chromatography, High Pressure Liquid MH - Drug Residues/*analysis MH - Food Contamination/*analysis MH - Milk/*chemistry MH - Tandem Mass Spectrometry EDAT- 2014/09/05 06:00 MHDA- 2015/09/02 06:00 CRDT- 2014/09/05 06:00 PHST- 2014/09/05 06:00 [entrez] PHST- 2014/09/05 06:00 [pubmed] PHST- 2015/09/02 06:00 [medline] AID - 10.3724/sp.j.1123.2013.12028 [doi] PST - ppublish SO - Se Pu. 2014 May;32(5):519-23. doi: 10.3724/sp.j.1123.2013.12028.