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12mL及8mL在60℃水浴中提取2次,每次10min。离心分离,合并2次提取液。向提取液中加入饱和硼砂溶液9mL和300g·L-1硫酸锌溶液3mL,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5mL水淋洗,弃去淋洗液。用甲醇-乙酸乙酯(10+90)混合液10mL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1.0mL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380nm。结果表明:喹乙醇的质量浓度在0.150～50.0mg·L-1内与其峰面积之间呈线性关系,检出限(3S/N)为30μg·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。
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 with10 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 CH3 OH-H2 O(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(3 S/N)of 30μg·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%.
作者
黄鸾玉
杨姝丽
韦信贤
童桂香
吴祥庆
黄玉柳
蒙源
HUANG Luanyu;YANG Shuli;WEI Xinxian;TONG Guixiang;WU Xiangqing;HUANG Yuliu;MENG Yuan(Guangxi Academy of Fishery Sciences,Natmifig 530021,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2019年第4期427-431,共5页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
广西重点研发项目(AB16380252)
关键词
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
