SPE净化HPLC-APCI(＋)-MS／MS分析肉类食品中硝基咪唑类药物原药及代谢物残留量  

Determination of Nitroimidazoles Drug Residues in Meat Products by HPLC-APCI(+)-MS/MS

作　　者：殷居易[1] 谢东华[1] 陈杰[1] 章再婷[1] 

机构地区：[1]宁波出入境检验检疫局技术中心,食品安全分析中心,浙江宁波315012

出　　处：《质谱学报》2009年第4期193-200,共8页Journal of Chinese Mass Spectrometry Society

基　　金：浙江宁波出入境检验检疫局科技资助项目(甬F09-2008)

摘　　要：采取固相萃取柱净化处理后进行液相色谱-大气压化学电离源串联四极杆质谱,在正离子检测模式下(HPLC-APCI(+)-MS/MS)对动物源性肉类食品中甲硝唑、地美硝唑(二甲硝唑)、替硝唑、洛硝唑(罗硝唑)、特尼哒唑、异丙硝唑、以及羟基化甲硝唑、羟基化异丙硝唑、2-羟甲基-1-甲基化-5-硝咪唑9种硝基咪唑类药物残留量进行分析。样品添加氘代标示物HMMNI-D3、IPZ-OH-D3后,用乙腈提取,通过OASISMCXC18SPE柱净化,SuperiorexODSC18色谱柱分离,采用梯度洗脱,流动相为0.1%甲酸水溶液和0.1%甲酸乙腈溶液,大气压电离源正离子MRM模式检测。肉类肌肉样品的方法定量下限(LOQ,S/N>10)为0.5μg.kg-1。在质量浓度0.5～100.0μg.L-1范围内,峰面积与浓度呈良好的线性关系(r:0.9971～0.9996)。An HPLC-APCI（＋）MS-MS methodology was developed coupled with solid phase extraction decontamination for the residue determination of nitroimidazoles, metronidazole （MNZ）, dimetridazole（DMZ）, tindazole（TNZ）, ronidazole（RNZ）, ternidazole（TerNDZ）, ipronidazole（IPZ）, hydroxy-metronidazole （MNZOH）, hydroxy-ipronidazole （IPZOH）, 2- hydroxymethyl-1-methyl-5-nitro-imidazole（HMMNI）. The sample was extracted with the acetonitrile followed by appending deuterium-marker （HMMNI-D^3 , IPZ-OH-D^3 ） internal standard, and operated for decontamination by OASIS MCX C18 cartridges. The chromatographic column was Superiorex ODS C18, the mobile phase was gradient solvent programming elution, which was consisted of water-acetic acid（0. 1%） and acetonitrile-acetic acid （0.1%）. Samples were ionized in flowing with a APCI ion source in positive mode, and were detected with MRM mode. The LOQ （S/N〉10） of nitroimidazoles residues in meat sample is 0.5μg·kg^-1. The response for nitroimidazoles is linear in the range of 0.5-100.0μg·L-1 , and the correlation coefficient is excellent（r= 0. 997 1-0. 999 6）.

关 键 词：高效液相色谱串联四极杆质谱 大气压电离源 硝基咪唑类药物 肉类食品 柱净化 

分 类 号：O657.63[理学—分析化学] S767.3[理学—化学]