摘要
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。
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.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2014年第8期1171-1176,共6页
Chinese Journal of Analytical Chemistry
基金
国家自然科学基金资助项目(No.50872042)资助~~
关键词
麻辣烫汤液
喹诺酮类抗生素
固相萃取
高效液相色谱
荧光检测
Spicy soup
Quinolones
Packed fiber solid phase extraction
High performance liquidchromatography
Fluorimetric detection
