Citation: LI Wei, AI Lianfeng, GUO Chunhai, MA Yusong, DOU Caiyun. Simultaneous determination of penicillin and their major enzymatic metabolites in milk and milk powder by high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2013, 31(10): 946-953. doi: 10.3724/SP.J.1123.2013.03016 shu

Simultaneous determination of penicillin and their major enzymatic metabolites in milk and milk powder by high performance liquid chromatography-tandem mass spectrometry

1.
Hebei Entry-Exit Inspection and Quarantine Bureau, Shijiazhuang 050051, China

Corresponding author: LI Wei,
Received Date: 6 March 2013
Available Online: 22 April 2013
Fund Project: 国家质检总局科技基金项目(2010IK126). (2010IK126)

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 β-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 μg/L to 200 μg/L for penicillins and from 10 μg/L to 500 μg/L for enzymatic metabolites. The limits of detection and the limits of quantification were 5-50 μg/kg (S/N≥3) and 8-100 μg/kg (S/N≥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.
- high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS),
- penicillin,
- enzymatic metabolites,
- milk,
- milk powder
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沈阳化工大学材料科学与工程学院沈阳 110142