Determination of Amantadine Residue in Honey by Solid-phase Extraction and High-performance Liquid Chromatography with Pre-column Derivatization and Fluorometric Detection  被引量:15

Determination of Amantadine Residue in Honey by Solid-phase Extraction and High-performance Liquid Chromatography with Pre-column Derivatization and Fluorometric Detection

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作  者:张金振 赵静 周金慧 薛晓峰 李熠 吴黎明 陈芳 

机构地区:[1]Bee Products Quality Supervision and Testing Center, Institute of Apicultural Research, Chinese Academy of Agricultural Sciences, Beijing 100093, China

出  处:《Chinese Journal of Chemistry》2011年第8期1764-1768,共5页中国化学(英文版)

摘  要:Amantadine (AMA) is an anti-viral drug used in apiculture to protect honeybee against the sacbrood virus (Morator aetatulae). This study described a reliable high-performance liquid chromatographic (HPLC) method for analyzing AMA in honey using a solid-phase extraction (SPE) cartridge (Plexa PCX) for purification, 4-fluoro-7- nitro-2,1,3-benzoxadiazole (NBD-F) as a pre-column derivatization agent, and fluorometric detection (λex =470 nm, λem=530 nm). The chromatographic separation was performed on an XDB C18 column (150×4.6 mm i.d.) using 0.1% trifluoroacetic acid/acetonitrile (35 ; 65, V/V) as the mobile phase at a flow rate of 1.0 mLomin 1 with a run time of 20 min. Under these optimal conditions, a linear relationship was observed in the range of 0.025--1.0μg·mL-1 with a good correlation coefficient (0.998) and low limit of detection (0.0080 μg·g-1), the recoveries were all above 90%, and the intra-day and inter-day precision (RSD) ranged from 3.4%--5.1%.Amantadine (AMA) is an anti-viral drug used in apiculture to protect honeybee against the sacbrood virus (Morator aetatulae). This study described a reliable high-performance liquid chromatographic (HPLC) method for analyzing AMA in honey using a solid-phase extraction (SPE) cartridge (Plexa PCX) for purification, 4-fluoro-7- nitro-2,1,3-benzoxadiazole (NBD-F) as a pre-column derivatization agent, and fluorometric detection (λex =470 nm, λem=530 nm). The chromatographic separation was performed on an XDB C18 column (150×4.6 mm i.d.) using 0.1% trifluoroacetic acid/acetonitrile (35 ; 65, V/V) as the mobile phase at a flow rate of 1.0 mLomin 1 with a run time of 20 min. Under these optimal conditions, a linear relationship was observed in the range of 0.025--1.0μg·mL-1 with a good correlation coefficient (0.998) and low limit of detection (0.0080 μg·g-1), the recoveries were all above 90%, and the intra-day and inter-day precision (RSD) ranged from 3.4%--5.1%.

关 键 词:AMANTADINE HONEY solid-phase extraction high-performance liquid chromatographic (HPLC) fluorometric detection 

分 类 号:O657.72[理学—分析化学] X132[理学—化学]

 

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