超高效液相色谱法同时测定水产品中的盐酸氯苯胍及其代谢产物  

Simultaneous determination of robenidine hydrochoride and its metabolites in aquatic products by UPLC

作　　者：刘永涛[1,2] 董靖 李乐[3] 杨秋红 杨移斌[1,2] 艾晓辉[1,2] 

机构地区：[1]中国水产科学研究院长江水产研究所,武汉430223 [2]淡水水产健康养殖湖北省协同创新中心,武汉430070 [3]中国水产科学研究院,北京100141

出　　处：《分析试验室》2017年第9期1058-1061,共4页Chinese Journal of Analysis Laboratory

基　　金：中国水产科学研究院基本科研业务费(2016HY-ZD1202;2016JBF0104);现代农业产业技术体系专项资金(CARS-49);公益性行业(农业)科研专项(201503108-CC-1)资助

摘　　要：建立了水产品肌肉组织中盐酸氯苯胍及其代谢物4-氯苯甲酰胺基乙酸、4-氯苯甲酸和4-氯苯甲醛同时测定的超高效液相色谱双波长分析法。样品经乙酸乙酯(含1%甲酸)提取,无水硫酸钠除水,正己烷除脂后在ACQUIT UPLC BEH C_(18)色谱柱上分离,250 nm和313 nm双波长测定。盐酸氯苯胍及其3种代谢产物在0.05~5.0 mg/L浓度范围内呈良好的线性关系,相关系数(r^2)均≥0.9982。在空白黄颡鱼、中华鳖、罗非鱼和团头鲂组织中进行0.10,0.50,1.0 mg/kg 3个水平的加标回收试验,4种待测物平均回收率为61.7%~104.6%,相对标准偏差为0.97%~9.8%。盐酸氯苯胍、4-氯苯甲酰氨基乙酸和4-氯苯甲酸的检出限(LOD)均为0.025 mg/kg,定量限(LOQ)均为0.05 mg/kg,4-氯苯甲醛的检出限(LOD)为0.05 mg/kg,定量下限(LOQ)为0.10 mg/kg。应用该方法研究了盐酸氯苯胍在团头鲂体内组织分布和消除规律。An originalmethod for the simultaneous determination of robenidine hydrochoride and its metabolites including（ 4-Chloro-benzoylamino）-acetic acid,4-chlorobenzldehyde and 4-chlorobenzoic in aquatic products was established by ultra high performance liquid chromatography（ UPLC） with dual wavelength ultraviolet detector. The sample was extracted using ethyl acetate containing 1%formic acid,and moisture of sample was removed with anhydrous sodium sulfate,then n-hexane was used for removing fat in sample. After that,the sample prepared was separated on an ACQUIT UPLC BEH C18 column and determined with dual wavelengths at 250 nm and 313 nm. Good linearities were observed in the range of 0. 05 - 5. 0 mg/L,and the correlation coefficients for 4 analytes were all not less than 0. 9982. The average recoveries of 4 analytes ranged from 61. 7% to 104. 6% at the spiked level of 0. 10 - 1. 0 mg/kg in Yellow catfish（ Pelteobagrus fulvidraco）,Chinese soft shell turtle（ Trionyx Sinensis）, Tilapia（ Tilapia nilotica） and Bluntnose black bream（ Megalobramaamblycephala） muscle tissue. The relative standard deviations（ RSDs） were in the range of 0. 97% -9. 8%. The detection limits（ LODs） and quantitation limits（ LOQs） for robenidine hydrochloride,（ 4-Chloro-benzoylamino）-acetic acid and 4-chlorobenzoic were all 0. 025 mg/kg and 0. 05 mg/kg,while for 4-chlorobenzldehyde was 0. 05 mg/kg and 0. 10 mg/kg,respectively. The present method was applied to study on the tissue distribution and depletion regularity in Bluntnose black bream for the first time.

关 键 词：水产品 盐酸氯苯胍 代谢物 双波长 超高效液相色谱 

分 类 号：TS201.6[轻工技术与工程—食品科学]