Zhou Jinhui, Xue Xiaofeng, Chen Fang, Zhang Jinzhen, Li Yi, Wu Liming, Chen Lanzhen, Zhao Jing
Bee Research Institute, Chinese Academy of Agricultural Sciences, Bee Product Quality Supervision and Testing Center, Ministry of Agriculture, Beijing, China.
J Sep Sci. 2009 Apr;32(7):955-64. doi: 10.1002/jssc.200800545.
A method for the quantitative determination of seven fluoroquinolone antibacterial agents (FQs) used in beekeeping, viz. ciprofloxacin, norfloxacin, ofloxacin, pefloxacin, danofloxacin, enrofloxacin, and difloxacin, in royal jelly samples was developed on the basis of high performance liquid chromatography with fluorescence detection. Sample preparation included deproteination, ultrasonic-assisted extraction with a mixed inorganic solution of monopotassium phosphate (KH(2)PO(4)) and ethylenediaminetetraacetic acid disodium salt (Na(2)EDTA), and clean-up on a solid-phase extraction cartridge. The extraction procedure was optimized with regard to the amount of inorganic solvent and the duration of sonication for royal jelly as a complicated matrix. Overall recoveries for FQs ranged from 85.9 to 99.1% for royal jelly with standard deviations between 2.79 and 6.27%. Limits of quantification were 2-40 ng/g for seven FQs in royal jelly. A total of 57 real royal jelly samples collected from beekeepers and supermarkets were analyzed. The three most abundant honeybee-use FQs, i. e. ofloxacin, ciprofloxacin, and norfloxacin, were determined in some royal jelly samples in concentrations ranging from 11.9 to 55.6 ng/g. Unexpectedly, however, difloxacin was found at concentrations of about 46.8 ng/g in one sample although it is rarely used in beekeeping. The presented method was successfully applied to quantify FQs in real royal jelly samples.
基于高效液相色谱-荧光检测法，建立了一种定量测定蜂王浆样品中7种养蜂用氟喹诺酮类抗菌剂（FQs）的方法，这7种抗菌剂分别为环丙沙星、诺氟沙星、氧氟沙星、培氟沙星、达氟沙星、恩诺沙星和二氟沙星。样品制备包括去蛋白、用磷酸二氢钾（KH(2)PO(4)）和乙二胺四乙酸二钠盐（Na(2)EDTA）的混合无机溶液进行超声辅助萃取，以及在固相萃取柱上进行净化。针对蜂王浆这种复杂基质，对无机溶剂用量和超声处理时间进行了萃取程序优化。蜂王浆中FQs的总回收率在85.9%至99.1%之间，标准偏差在2.79%至6.27%之间。蜂王浆中7种FQs的定量限为2 - 40 ng/g。共分析了57份从养蜂人和超市采集的真实蜂王浆样品。在一些蜂王浆样品中检测到了三种使用最多的蜜蜂用FQs，即氧氟沙星、环丙沙星和诺氟沙星，其浓度范围为11.9至55.6 ng/g。然而，出乎意料的是，在一个样品中发现二氟沙星的浓度约为46.8 ng/g，尽管它在养蜂中很少使用。所提出的方法成功应用于定量真实蜂王浆样品中的FQs。
