色谱Issue(6):640-646,7.
复合免疫亲和柱净化-液相色谱-串联质谱法同时测定动物源性食品中6种玉米赤霉醇类化合物和氯霉素残留量
Simultaneous determination of zeranols and chloramphenicol in foodstuffs of animal origin by combination immunoaffinity column clean-up and liquid chromatography-tandem mass spectrometry
摘要
Abstract
A combination immunoaffinity column( IAC-CZ)clean-up and liquid chromatogra-phy-tandem mass spectrometry(LC-MS / MS)analytical method was successfully developed for the simultaneous determination of zeranols( ZER,α-zearalanol,β-zearalanol,zearalanone,α-zearalenol,β-zearalenol and zearalenone)and chloramphenicol( CAP)in foodstuffs of animal origin. The samples(fish,liver,milk and honey)were enzymatically digested by β-glucuroni-dase / sulfatase for about 16 h and then extracted with ether. The extracts were evaporated to dryness and then the residues were dissolved by 1.0 mL of 50% acetonitrile solution. After fil-tered and diluted with PBS buffer,the reconstituted solution were cleaned-up with a IAC-CZ and then analyzed by LC-MS / MS in multiple reaction monitoring(MRM)mode. The chromato-graphic separation was performed on a Shimadzu Shim-pack VP-ODS column with gradient elu-tion by acetonitrile and 2 mmol / L ammonium acetate solution. The detection was carried out by electrospray negative ionization mass spectrometry in MRM mode. The proposed method was validated by the limit of detection(0. 04-0. 10 μg / kg),linearity(R 2≥0. 999 0),average recov-eries(70. 9% -95. 6% )and precisions(2. 0% -11. 8% ). The developed method is reliable,sensi-tive and has good applicability. The combination immunoaffinity column was proved to be an effective pretreatment technique to decrease the matrix effect,and it met the requirements of residue analysis of co-occurring zeranols and chloramphenicol.关键词
复合免疫亲和柱/液相色谱-串联质谱/玉米赤霉醇类化合物/氯霉素/动物源性食品Key words
combination immunoaffinity column/liquid chromatography-tandem mass spec-trometry(LC-MS / MS)/zeranols/chloramphenicol/foodstuffs of animal origin分类
化学化工引用本文复制引用
王清,王国民,郗存显,李贤良,陈冬东,唐柏彬,张雷,赵华..复合免疫亲和柱净化-液相色谱-串联质谱法同时测定动物源性食品中6种玉米赤霉醇类化合物和氯霉素残留量[J].色谱,2014,(6):640-646,7.基金项目
科技部质检公益项目(201210086). ()