HPLC Determination of R-fenoxaprop-p-ethyl with Eggshell Membrane Solid Phase Extraction
摘 要
采用蛋壳膜固相萃取-高效液相色谱法测定除草剂R-精噁唑禾草灵的含量。优化的试验条件如下:① 固相萃取时间为80 min;② 洗脱剂甲醇的用量为1 mL;③ 样品溶液的酸度为pH 7;④ 样品溶液的体积为25~100 mL。以C18色谱柱为分离柱,以甲醇-水(80+20)混合液为流动相,在检测波长236 nm处进行测定。R-精噁唑禾草灵质量浓度在5.00~50.0 μg·L-1范围内与峰面积呈线性关系,方法检出限(3S/N)为1.2 μg·L-1。方法用于水样和小麦粉样品分析,加标回收率在75.4%~95.2%之间,测定值的相对标准偏差(n=5)在3.7%~5.8%之间。
Abstract
HPLC with eggshell membrane solid phase extraction was applied to the determination of the herbicide R-fenoxaprop-p-ethyl. The optimized conditions found were as follows: ① time of solid phase extraction was 80 min; ② amount of methanol used as eluent was 1 mL; ③ acidity of sample solution was pH 7; ④ volume of sample solution was 25 to 100 mL. C18 chromatographic column was used as stationary phase, and a mixture of methanol and water (80+20) was used as mobile phase. UV-detection at 236 nm was adopted in the determination. Linear relationship between values of peak area and mass concentration of R-fenoxaprop-p-ethyl was kept in the range of 5.00-50.0 μg·L-1, with detection limit (3S/N) of 1.2 μg·L-1. The proposed method was applied to the analysis of samples of water and wheat powder, giving values of recovery and RSD′s (n=5) in the ranges of 75.4%-95.2% and 3.7%-5.8% respectively.
中图分类号 O652.63
所属栏目 工作简报
基金项目 青岛农业大学高层次人才启动基金(630736)
收稿日期 2013/3/23
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联系人作者赵艳芳(qndxlb@163.com)
备注赵艳芳(1978-),女,山东聊城人,副教授,博士,主要研究方向为光谱、色谱分析。
引用该论文: ZHAO Yan-fang,XU Lu-bin,SONG Ji-ying. HPLC Determination of R-fenoxaprop-p-ethyl with Eggshell Membrane Solid Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2014, 50(5): 583~585
赵艳芳,徐鲁斌,宋吉英. 蛋壳膜固相萃取-高效液相色谱法测定R-精噁唑禾草灵[J]. 理化检验-化学分册, 2014, 50(5): 583~585
被引情况:
【1】赵艳芳,朱国强,徐鲁斌, "蛋壳膜负载双硫腙吸附富集-火焰原子吸收光谱法测定饮用水中镉",理化检验-化学分册 52, 176-178(2016)
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参考文献
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【2】吕波,艾萍,李俊,等.麦田蔺草对精噁唑禾草灵的抗性研究[J].南京农业大学学报, 2012,35(1):57-62.
【3】韩玉,汪兰,孙智达,等.蛋壳及蛋壳膜吸附性质的研究进展[J].食品工业科技, 2012,33(13):388-391.
【4】PUNDIR C S, BHAMBI M, CHAUHAN N S. Chemical activation of egg shell membrane for covalent immobilization of enzymes and its evaluation as inert support in urinary oxalate determination[J]. Talanta, 2009,77(5):1688-1693.
【5】LI Bao-xin, LAN Dan, ZHANG Zhu-jun. Chemiluminescence flow-through biosensor for glucose with eggshell membrane as enzyme immobilization platform[J]. Analytical Biochemistry, 2008,374:64-70.
【6】MINE Y, OBERLE C, KASSAIFY Z. Eggshell matrix proteins as defense mechanism of avian eggs[J]. Journal of Agricultural and Food Chemistry, 2003,51:249-253.
【7】TSAIA W T, YANGB J M, LAIA C W, et al. Characterization and adsorption properties of eggshells and eggshell membrane[J]. Bioresource Technology, 2006,97(3):488-493.
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