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超高效液相色谱法测定水产品中喹乙醇的残留量
          
Determination of Residual Amounts of Olaquindox in Aquatic Products by UPLC

摘    要
称取经粉碎并匀浆后的水产样品(5.00±0.05)g,先后用水12 mL及8 mL在60℃水浴中提取2次,每次10 min。离心分离,合并2次提取液。向提取液中加入饱和硼砂溶液9 mL和300 g·L-1硫酸锌溶液3 mL,充分混匀进行脱色和除去杂质。离心分离,取上清液,通过固相萃取柱(SPE)使被测组分吸附在柱上,SPE柱用5 mL水淋洗,弃去淋洗液。用甲醇-乙酸乙酯(10+90)混合液10 mL将被测组分从柱上洗脱。收集洗脱液并在50℃条件下吹氮至近干,残渣用色谱分离所用的流动相1.0 mL溶解,以下按色谱条件操作。用BEH C18色谱柱为固定相,甲醇-水(15+85)混合液为流动相进行色谱分离;用紫外检测器,检测波长为380 nm。结果表明:喹乙醇的质量浓度在0.150~50.0 mg·L-1内与其峰面积之间呈线性关系,检出限(3S/N)为30 μg·kg-1。用标准加入法进行回收试验,测得回收率在76.4%~90.2%之间,测定值的相对标准偏差(n=5)在3.3%~9.0%之间。
标    签 超高效液相色谱法   紫外检测器   喹乙醇   水产品   ultra high performance liquid chromatography   ultraviolet detector   olaquindox   aquatic product  
 
Abstract
Aquatic sample was minced, pulped and homogenized to a gruel-like state. A portion (5.00±0.05) g of the sample was taken and extracted twice with 12 mL and 8 mL of water at 60℃ for 10 min in each extraction. After centrifuging, the extracts were combined, decolorized and separated from some impurities by mixing with 9 mL of saturated borax solution and 3 mL of 300 g·L-1 zinc sulfate solution. The mixture was centrifugated, and the supernatant was taken and passed through SPE column to have the analyte (OLA) adsorbed on the column. The column was rinsed with 5 mL of water which were discarded. Then the column was eluted with 10 mL of a mixture of methanol and ethyl acetate (10+90) to desorb OLA from the column. The eluate was collected and evaporated to near dryness by N2-blowing at 50℃. The residue was dissolved with 1.0 mL of the mobile phase used in UPLC analysis, and the solution was used for UPLC separation and determination. BEH C18 column was used as the stationary phase and a mixture of CH3OH-H2O (15+85) was used as mobile phase in the LC separation. UV detector was used in the detection at the wavelength of 380 nm. Linear relationship between values of peak area and mass concentration of OLA in the range of 0.150-50.0 mg·L-1 was obtained, with detection limit (3S/N) of 30 μg·kg-1. Recovery was tested by standard addition method, giving values of recovery ranged from 76.4% to 90.2%. Values of RSDs (n=5) were found in the range of 3.3%-9.0%.

中图分类号 O657.7   DOI 10.11973/lhjy-hx201904010

 
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所属栏目 工作简报

基金项目 广西重点研发项目(AB16380252)

收稿日期 2018/7/19

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备注黄鸾玉,工程师,硕士研究生,主要从事渔业环保及水产品质量安全检测技术研究工作,huangluanyu@163.com

引用该论文: HUANG Luanyu,YANG Shuli,WEI Xinxian,TONG Guixiang,WU Xiangqing,HUANG Yuliu,MENG Yuan. Determination of Residual Amounts of Olaquindox in Aquatic Products by UPLC[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2019, 55(4): 427~431
黄鸾玉,杨姝丽,韦信贤,童桂香,吴祥庆,黄玉柳,蒙源. 超高效液相色谱法测定水产品中喹乙醇的残留量[J]. 理化检验-化学分册, 2019, 55(4): 427~431


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