Simultaneous Determination of Tetracylines and Quinolones Antibiotics in Egg by Ultra-Performance Liquid Chromatography-Electrospray Tandem Mass Spectrometry

Abstract We report here an ultra-performance liquid chromatography coupled with tandem mass spectrometric (MS/MS) method for the simultaneous quantitation of multiclass veterinary drugs in egg. The analysis of the target compounds, including 7 tetracyclines and 4 types of quinolones, may be accomplished in 15 min of total run time. The egg was extracted with ethylenediaminetetraacetic acidMcIlvaine buffer solution and further purified using a polymer-based Oasis HLB solid-phase extraction cartridge. A C18 column was used to separate the analytes followed by MS/MS using an electrospray ion source. The overall average recoveries of the analytes based on matrix-fortified calibration ranged from 71 to 112 with acceptable relative standard deviations of <20 for 6 trials. For all of the target compounds, the limits of quantitation ranged between 0.02 and 4.29 g/kg. The proposed method is sufficiently sensitive and highly selective.

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Validation of a Solid-Phase Extraction and Ultra-Performance Liquid Chromatographic Tandem Mass Spectrometric Method for the Detection of 16 Glucocorticoids in Pig Tissues

Journal of AOAC International ◽

10.1093/jaoac/92.2.604 ◽

2009 ◽

Vol 92 (2) ◽

pp. 604-611 ◽

Cited By ~ 13

Author(s):

Bing Shao ◽

Xiaoliang Cui ◽

Yi Yang ◽

Jing Zhang ◽

Yongnin Wu

Keyword(s):

Solid Phase Extraction ◽

Solid Phase ◽

Monitoring Program ◽

Ion Source ◽

Tandem Mass ◽

Phase Extraction ◽

Mass Spectrometric Method ◽

Relative Standard ◽

Liver And Kidney ◽

Tandem Mass Spectrometric

Abstract A sensitive analytical method has been developed and validated for simultaneous determination of 16 glucocorticoid (fluorometholone, flumethasone, triamcinolone, aldosterone, clobetasol propionate, methylprednisolone, fluocinolone acetonide, hydrocortisone, prednisone, dexamethasone, beclomethasone, prednisolone, budesonide, triamcinolone acetonide, fludrocortisone acetate, and cortisone) residues in pig tissues (muscle, liver, and kidney). These biosamples were hydrolyzed with -glucuronidase/arylsulfatase enzyme and passed through a Supelclean ENVI-Carb graphitized carbon black solid-phase extraction cartridge, followed by further purification using aminopropyl cartridges. Analytes were separated on an ultra-performance liquid chromatography BEH C18 column followed by tandem mass spectrometry (MS) with an electrospray ion source. The MS data acquisition was performed in the negative multireaction monitoring mode by a time-scheduled multireaction monitoring program. The assay for the 16 glucocorticoids were linear over the range of 1250 g/L for pork, liver, and kidney, with correlation coefficient >0.99. Estimated detection limits for the target analytes ranged from 0.03 to 0.30 g/kg, and limits of quantitation ranged from 0.10 to 1.00 g/kg. Recoveries of the glucocorticoids (spiked at levels of 0.4 and 2.0 g/kg) ranged from 81.0 to 112.3, with relative standard deviations between 2.6 and 16.6.

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Simultaneous Determination of 16 Sulfonamides in Honey by Liquid Chromatography/TandemMass Spectrometry

Journal of AOAC International ◽

10.1093/jaoac/88.5.1304 ◽

2005 ◽

Vol 88 (5) ◽

pp. 1304-1311 ◽

Cited By ~ 17

Author(s):

Guo-Fang Pang ◽

Yan-Zhong Cao ◽

Jin-Jie Zhang ◽

Guang-Qun Jia ◽

Chun-Lin Fan ◽

...

Keyword(s):

Liquid Chromatography ◽

Solid Phase ◽

Phosphoric Acid Solution ◽

Tandem Mass ◽

Phase Extraction ◽

Chromatography Tandem Mass Spectrometry ◽

Relative Standard ◽

Liquid Chromatography Tandem Mass ◽

Oasis Hlb

Abstract A method is described for the determination of 16 sulfonamides in honey. Samples are dissolved in phosphoric acid solution (pH2), cleaned up with 2 solid-phase extraction (SPE) cartridges, an aromatic sulfonic cation-exchange cartridge and an Oasis HLB SPE cartridge, and analyzed both qualitatively and quantitatively by liquid chromatography/tandem mass spectrometry (LC/MS/MS) under the selected conditions. Without exception, calibration curves were linear (r = >0.995), when sulfamethizole was between 1.0 and 25.0 μg/kg; sulfacetamide, sulfapyridine, sulfadiazine, sulfachloropyridazine, sulfamethoxazole, sulfamerazine, sulfisoxazole, sulfamonomethoxine, and sulfadoxine were between 2.0 and 50.0 μg/kg; sulfamethoxypyridazine, sulfadimethoxine, and sulfathiazole were between 4.0 and 100.0 μg/kg; sulfamethazine and sulfameter were between 8.0 and 200.0 μg/kg; and sulfaphenazole was between 12.0 and 300.0 μg/kg. Average recoveries at 4 fortification levels in the range of 1.0–300 μg/kg in honey were 70.9–102.5%, and relative standard deviations were 2.02–11.52%. The limits of quantitation for the 16 sulfonamides were between 1.0 and 12.0 μg/kg, with the LC/MS/MS method.

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