PMID- 24432636 OWN - NLM STAT- MEDLINE DCOM- 20150708 LR - 20190923 IS - 1000-8713 (Print) IS - 1000-8713 (Linking) VI - 31 IP - 10 DP - 2013 Oct TI - [Simultaneous determination of penicillin and their major enzymatic metabolites in milk and milk powder by high performance liquid chromatography-tandem mass spectrometry]. PG - 946-53 AB - A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/ MS) method has been developed for the determination of eight compounds in milk and milk powder. They are four penicillins (penicillin G, penicillin V, amoxicillin and ampicillin) and four major beta-lactamase enzymatic metabolites of them (penilloic acid G, penilloic acid V, amoxiilloic acid and ampilloic acid). The compounds were extracted from the samples with acetonitrile and water, cleaned-up by HLB solid-phase extraction cartridges, and then detected by HPLC-MS/MS and quantified by external standard method. The linearities were satisfactory with the correlation coefficients > 0.99 at the mass concentrations ranging from 4 microg/L to 200 microg/L for penicillins and from 10 microg/L to 500 microg/L for enzymatic metabolites. The limits of detection and the limits of quantification were 5-50 microg/kg (S/N > or = 3) and 8-100 microg/kg (S/N > or = 10), respectively. The average recoveries of the eight compounds were 83.48%-96.97% in milk and 82.70%-95.14% in milk powder. The relative standard deviations (RSDs) in milk and milk powder were 3.86%-10.87% and 3.02%-9.81%, respectively. In conclusion, the established method is convenient, accurate and sensitive so that it can be applied to the determination of penicillin residues and enzymatic metabolites in milk and milk powder. FAU - Li, Wei AU - Li W AD - Hebei Entry-Exit Inspection and Quarantine Bureau, Shijiazhuang 050051, China. liwei.305@163.com FAU - Ai, Lianfeng AU - Ai L AD - Hebei Entry-Exit Inspection and Quarantine Bureau, Shijiazhuang 050051, China. FAU - Guo, Chunhai AU - Guo C AD - Hebei Entry-Exit Inspection and Quarantine Bureau, Shijiazhuang 050051, China. FAU - Ma, Yusong AU - Ma Y AD - Hebei Entry-Exit Inspection and Quarantine Bureau, Shijiazhuang 050051, China. FAU - Dou, Caiyun AU - Dou C AD - Hebei Entry-Exit Inspection and Quarantine Bureau, Shijiazhuang 050051, China. LA - chi PT - Journal Article PL - China TA - Se Pu JT - Se pu = Chinese journal of chromatography JID - 9424804 RN - 0 (Penicillins) RN - 0 (Powders) RN - 804826J2HU (Amoxicillin) RN - F93JSF8762 (penilloic acid) RN - Q42T66VG0C (Penicillin G) SB - IM MH - Amoxicillin MH - Animals MH - Chromatography, High Pressure Liquid MH - Drug Residues/*analysis MH - Food Contamination/*analysis MH - Mass Spectrometry MH - Milk/*chemistry MH - Penicillin G/analogs & derivatives MH - Penicillins/*analysis MH - Powders MH - Solid Phase Extraction MH - *Tandem Mass Spectrometry EDAT- 2014/01/18 06:00 MHDA- 2015/07/15 06:00 CRDT- 2014/01/18 06:00 PHST- 2014/01/18 06:00 [entrez] PHST- 2014/01/18 06:00 [pubmed] PHST- 2015/07/15 06:00 [medline] AID - 10.3724/sp.j.1123.2013.03016 [doi] PST - ppublish SO - Se Pu. 2013 Oct;31(10):946-53. doi: 10.3724/sp.j.1123.2013.03016.