| 摘要: |
| 以南美白对虾为试验材料，建立了喹乙醇（OLA）及3-甲基-喹恶啉-2-羧酸（MQCA）多残留的高效液相色谱-串联质谱（HPLC-MS/MS）确证检测法。组织样品经2 mol/L盐酸提取，Oasis HLB固相萃取柱净化，采用HPLC-MS/MS仪进行测定。质谱检测采用正离子选择反应监测模式，外标法定量。样品中OLA和MQCA质量分数分别为2~200和4~200 μg/kg时，线性关系良好；当质量分数分别为2~50和4~50 μg/kg时，平均回收率为93.9%~103.2%，变异系数为6.3%~11.5%。OLA及MQCA的检测限分别为0.5和1.0 μg/kg，定量限分别为2.0和4.0 g/kg。该方法灵敏、准确、简便、快速，适于南美白对虾中OLA及MQCA残留的同时定量分析和确证检测。 |
| 关键词: 南美白对虾 喹乙醇 3-甲基-喹恶啉-2-羧酸 残留 高效液相色谱-串联质谱 |
| DOI：10.11841/j.issn.1007-4333.2014.01.22 |
| 投稿时间：2013-07-03 |
| 基金项目:2013年无公害农产品质量安全监测项目资金（农财发[2013]86号） |
|
| Determination of residual olaquindox and methyl-3-quinoxaline-2-carboxylic acid in penaeus vannamei by HPLC-MS/MS |
|
GUO Xia, SUN Zhen-zhong, QI Jun-yuan, SUN Jian-hua, HUANG Xue-ling, LIU Qin, DING Yi
|
| (Shanghai Fisheries Research Institute, Shanghai 200433, China) |
| Abstract: |
| A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) determination of Olaquindox and methyl-3-quinoxaline-2-carboxylic acid in Penaeus vannamei muscle was established.Samples were extracted with 2 mol/L hydrochloric acid and clean-up was performed on a HLB solid-phase extraction cartridge.The residues were detected by HPLC-MS/MS.The identification was performed by selective reaction monitoring in positive electrospray ionization.The quantification was done by external standard method.Calibration curves were linear for OLA and MQCA in samples at 2-200 and 4-200 μg/kg respectively.At the fortified levels of 2-50 and 4-50 μg/kg,the recoveries ranged from 93.9% to 103.2%,coefficents of variation (CV) ranged from 6.3% to 11.5%.The limit of detection (LOD) of OLA and MQCA was 0.5 and 1.0 μg/kg respectively and the limit of quantitation (LOQ) was 2.0 and 4.0 μg/kg respectively.The results show that the method is sensitive,accurate,convenient and quick,which can be used to analyze simultaneously OLA and MQCA residues in penaeus vannamei muscle. |
| Key words: penaeus vannamei olaquindox methyl-3-quinoxaline-2-carboxylic acid residue high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) |
