Simultaneous determination of lincomycin and spectinomycin residues in animal tissues by gas chromatography-nitrogen phosphorus detection and gas chromatography-mass spectrometry with accelerated solvent extraction.
A new multi-dimensional analytical method using gas chromatography-nitrogen phosphorus detection (GC-NPD) and gas chromatography-mass spectrometry (GC-MS) was developed for qualitative and quantitative measurement of lincomycin and spectinomycin residues in food animal tissues. This method is based on a new extraction procedure using accelerated solvent extraction (ASE). The analytes were extracted by phosphate buffer with trichloroacetic acid deproteinization and clean-up by C₁₈ solid-phase extraction (SPE) adding dodecanesulfonic acid sodium salt as an ion-pair reagent. The eluted fraction was evaporated and derivatised with N,O-bis(trimethylsilyl) trifluoroacetamide (BSTFA) for GC-NPD analysis and GC-MS confirmation. Parameters for extraction pressure, temperature and cycle of ASE, clean-up, derivatisation and analysis procedure were optimised. The method was validated in muscle, kidney and liver of swine, bovine with a low concentration (limit of quantification) of 16.4 and 21.4 µg kg⁻¹ for these two analytes using GC-NPD. For GC-MS, the limits of quantification were 4.1 and 5.6 µg kg⁻¹, respectively. Spiked recoveries from levels of 20 to 200 µg kg⁻¹ were found to be between 73% and 99% with a relative standard deviation (RSD) of less than 17% in GC-NPD. For GC-MS, levels from 5 to 20 µg kg⁻¹ had between 70% and 93% with an RSD of less than 21%. This rapid and reliable method can be used for the characterisation and quantification of residues of lincomycin and spectinomycin in animal tissues.
National Reference Laboratory of Veterinary Drug Residues & MOA Key Laboratory of Food Safety Evaluation, Huazhong Agricultural University, Wuhan 430070, China.
Y
Y
Tao
D
D
Chen
G
G
Yu
H
H
Yu
Y
Y
Pan
Y
Y
Wang
L
L
Huang
Z
Z
Yuan
D053000:Analytic Sample Preparation Methods; D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis*; D002417:Cattle; D002849:Chromatography, Gas; D004350:Drug Residues / Q000032:analysis* / Q000737:chemistry / Q000592:standards; D005506:Food Contamination; D008401:Gas Chromatography-Mass Spectrometry; D006358:Hot Temperature; D007668:Kidney / Q000737:chemistry; D057230:Limit of Detection; D008034:Lincomycin / Q000032:analysis* / Q000737:chemistry; D008099:Liver / Q000737:chemistry; D008460:Meat / Q000032:analysis*; D018482:Muscle, Skeletal / Q000737:chemistry; D011312:Pressure; D015203:Reproducibility of Results; D052616:Solid Phase Extraction; D000198:Spectinomycin / Q000032:analysis* / Q000737:chemistry; D034421:Sus scrofa
D000900:Anti-Bacterial Agents; D000198:Spectinomycin; D008034:Lincomycin