title: [Determination of clavulanic acid residue in milk by high performance liquid chromatography-tandem mass spectrometry].
abstract: An analytical method was developed for the determination of clavulanic acid (CLAV) in milk by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). A 2 g milk sample was deproteinized by ethanol. The supernatant was transferred into a pear-shaped bottle to be evaporated to about 0.5 mL, and the residue was dissolved with ammonium acetate solution. The sample was determined by HPLC-MS/MS after the purification. The chromatographic separation was achieved on a Luna 5u C8 column using 0.1% formic acid in water and acetonitrile as mobile phases with gradient elution. The identification of CLAV was carried out by MS/MS equipped with electrospray ionization in negative scanning and multiple reaction monitoring (MRM) modes. Matrix-matched calibration standard was used for the quantification. The calibration curve showed perfect linear in the range of 10 - 400 microg/kg with the correlation coefficient of 0.999. The limit of detection (LOD, S/N > or = 3) was 10 microg/kg in milk, and the limit of quantification (LOQ, S/N > or = 10) was 20 microg/kg. The mean recoveries varied from 80.00% to 91.25% at the four spiked levels of LOQ, 1/2MRL (the maximum residue limit), MRL, and 2MRL with the relative standard deviations of 5.60% -8.77%. In conclusion, the established method can be applied for the determination of CLAV residues in milk.
authors.affiliation: National Reference Laboratory of Veterinary Drug Residues (SCAU), South China Agricultural University, Guangzhou 510642, China.
authors.forename: Gang
authors.initials: G
authors.lastname: Yang
authors.forename: Xianhui
authors.initials: X
authors.lastname: Huang
authors.forename: Chunna
authors.initials: C
authors.lastname: Guo
authors.forename: Qiuhua
authors.initials: Q
authors.lastname: Fang
authors.forename: Limin
authors.initials: L
authors.lastname: He
mesh_terms: D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis; D002417:Cattle; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D019818:Clavulanic Acid / Q000032:analysis*; D004350:Drug Residues / Q000032:analysis*; D005506:Food Contamination / Q000032:analysis; D013058:Mass Spectrometry / Q000379:methods*; D008892:Milk / Q000737:chemistry*
chemical_list: D000900:Anti-Bacterial Agents; D019818:Clavulanic Acid