• Korean Journal of Veterinary Service
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• v.42 no.4
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• pp.289-296
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• 2019

A novel rapid procedure with liquid chromatography tandem mass spectrometry (LC-MS/MS) detection has been developed by changing various conditions including sample preparation such as QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) methodology. This work has been involved the optimization and validation of detection method for fluoroquinolones which are widespread used in livestock especially in the chicken. Five grams of homogenized chicken muscle were extracted with QuEChERS EN and acetonitrile containing 5% formic acid and cleaned with anhydrous magnesium sulfate and C₁₈ sorbent. The separation was performed on Acquity UPLC HSS T3 (2.1 mm×100 mm, 1.8 ㎛) column. The mobile phase A and B were composed of water containing 0.1% formic acid and acetonitrile containing 0.1% formic acid, respectively. Flow rate was 0.25 mL/min and column temperate was 40℃. LC-MS/MS with multiple reaction monitoring has been optimized for ten fluoroquinolones (ciprofloxacin, danofloxacin, difloxacin, enrofloxacin, marbofloxacin, norfloxacin, ofloxacin, orbifloxacin, pefloxacin and sarafloxacin). The method developed in this study has been presented good linearity with correlation coefficient (R²) of 0.9971~0.9998. LOD and LOQ values ranged from 0.09 to 0.76 ppb and from 0.26 to 2.29 ppb, respectively. The average recoveries were from 77.46 to 111.83% at spiked levels of 10.0 and 20.0 ㎍/kg. Relative standard deviation (%) ranged 1.28~11.90% on intra-day and 3.10~8.38 % on inter-day, respectively. This analysis method was applicable to the livestock residue laboratories and was expected to be satisfactory for the residue surveillance system.

• Korean journal of food and cookery science
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• v.22 no.6 s.96
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• pp.774-782
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• 2006

Flavor components in fresh Codonopsis lanceolata cultivated on a wild hill were detected by headspace sampling(HSS) method and GC-MS equipped with a VB-5(5% phenylmethyl polysiloxane) column. The 167 volatile compounds that were detected, consisted of 28 terpenes and terpene alcohols, 34 hydrocarbon, 31 alcohols, 13 aldehydes and ketones, 25 esters, 6 acids, 10 ethers and 20 miscellaneous components. The ten major volatile flavor components, comprising about 58% of the total, were dl-limonene (10.2%), ${\alpha}$-guaiene (9.0%), 2,2,6-trimethyl-octane (8.6%), hexadecane (8.0%), isolongifolan-8-ol (4.2%), 2,4,4-trimethyl-1,3-pentanediol diisobutyrate (4.1%), ${\beta}$-selinene (3.9%), 2,2,3-trimethylnonane (3.6%), 3-methyl-5-propyl-nonane (3.1%), and ledene (3.1%). The unique aroma of fresh Codonopsis lanceolata described by sensory evaluation was green, earthy, camphoraceous and aldehydic. The components attributed to green or camphoraceous flavor such as 1-hexanol, 2-methylhexan-3-ol, 3-hexen-1-ol, cis-3-hexenyl butyrate, ethylhexanol, hexyl acetate, trans-2-hexen-1-ol, camphor, longiborneol and menthol were not included in the ten or twenty major volatile components which had the largest peak area in descending order. We concluded that the intensity of green and camphoraceous flavor might be used as an indicator of the freshness of Codonopsis lanceolata.