CAJ | 학술논문

建立了固相萃取-高效液相色谱-荧光检测麻辣烫汤液中5种喹诺酮类抗生素的分析方法。麻辣烫汤液样品经EDTA-Mcllvaine缓冲溶液(pH 4)提取后,以HCX固相萃取小柱净化富集,用水淋洗,2%氨化甲醇洗脱。采用高效液相色谱-荧光检测器( HPLC-FLD),于激发波长280 nm,发射波长450 nm处进行检测,流动相为甲醇-水-磷酸(25：75：0.1, V/V,三乙胺调至pH 2.8)。麻辣烫汤液样品中氟罗沙星、诺氟沙星、沙拉沙星、环丙沙星、奥比沙星5种喹诺酮类抗生素加标回收率为72.1%~110.3%；日内相对标准偏差( RSD)为1.6%~4.3%,日间相对标准偏差为2.0%~4.3%；检出限(LOD)为1.2~5.4μg/L；定量限(LOQ)为3.9~18μg/L。本方法能够满足实际麻辣烫汤液样品的分析要求。
건립료고상췌취-고효액상색보-형광검측마랄탕탕액중5충규낙동류항생소적분석방법。마랄탕탕액양품경EDTA-Mcllvaine완충용액(pH 4)제취후,이HCX고상췌취소주정화부집,용수림세,2%안화갑순세탈。채용고효액상색보-형광검측기( HPLC-FLD),우격발파장280 nm,발사파장450 nm처진행검측,류동상위갑순-수-린산(25：75：0.1, V/V,삼을알조지pH 2.8)。마랄탕탕액양품중불라사성、낙불사성、사랍사성、배병사성、오비사성5충규낙동류항생소가표회수솔위72.1%~110.3%；일내상대표준편차( RSD)위1.6%~4.3%,일간상대표준편차위2.0%~4.3%；검출한(LOD)위1.2~5.4μg/L；정량한(LOQ)위3.9~18μg/L。본방법능구만족실제마랄탕탕액양품적분석요구。
An analytical method for simultaneous determination of five quinolones in spicy soup was developed. Spicy soup samples were firstly extracted by EDTA-Mcllvaine buffer at pH 4, then purified and concentrated by a novel Packed fiber solid phase extraction ( PFSPE ) coulumn. The extracted liquid supernatant was loaded onto the column, rinsed with water, and then eluted with 2% ammoniated methanol. The mobile phase was methanol-water-phosphoric acid (25:75:0. 1, V/V, adjusting the pH to 2. 8 with triethylamine) . These analytes were quantified by high performance liquid chromatography-fluorimetric detector( HPLC-FLD) at excitation and emission wavelength of 280 nm and 450 nm respectively. Recoveries of spiked quinolone antibiotics in spicy soup were from 72 . 1% to 110 . 3% with intraday relative standard deviation (RSD) between 1. 6% and 4. 3% and inter-day RSD from 2. 0% to 4. 3%. Limit of detection (LOD) and limit of quantitation(LOQ) were from 1. 2 to 5. 4 μg/L and from 3. 9 to 18 μg/L, respectively. The method could be applied to determine the quinolones in spicy soup.