| 引用本文: | 梅景良,吴聪明,程林丽,沈建忠,薛 麒,钱民怡,邵梦瑜.HPLC 法同步检测鲤鱼、对虾中喹乙醇与MQCA 残留[J].海洋科学,2011,35(11):41-47. |
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| 摘要: |
| 建立了一种高效液相色谱法同时检测鲤鱼、对虾肌肉组织中喹乙醇(OLA)及其代谢物3-甲基-喹啉-2-羧酸(MQCA)的残留。采用0.3 mol/L 盐酸提取鲤鱼、对虾中的残留物, C18 固相萃取柱净化, 氮气吹干及流动相定容后, Waters2695 高效液相色谱仪在320 nm(MQCA)和372 nm(QLA)双波长同步检测,流动相由纯水、乙腈、甲醇和0.5%甲酸水组成, 梯度洗脱, 流速为1.0 mL/min, 外标法定量。在此条件下, 当OLA 及MQCA 在鱼组织中的添加水平分别为20～200 μg/kg 和35～200 μg/kg 时, 其平均回收率相应为83.5%～87.7%和79.6%～87.4%; 当OLA 及MQCA 在虾组织中的添加水平分别为15～200 μg/kg和30～200 μg/kg 时, 其平均回收率相应为74.6%～80.9%和81.0%～86.6%。两种动物组织中两种化合物的批内相对标准偏差RSD(n=5)为0.51%～4.47%, 批间相对标准偏差RSD(n=3)为0.66%～7.58%。鲤鱼组织中OLA 和MQCA 的检测限分别为6 μg/kg 和10 μg/kg, 定量限分别为20 μg/kg 和35 μg/kg; 对虾组织中OLA 和MQCA 的检测限分别为4.5 μg/kg 和8 μg/kg, 定量限分别为15 μg/kg 和30 μg/kg。 |
| 关键词: 喹乙醇 3-甲基-喹啉-2-羧酸 残留 高效液相色谱 鲤鱼 对虾 |
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| 基金项目:国家公益性行业(农业)科研专项经费资助(200903055) |
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| Simultaneous determination of olaquindox and MQCA in carp and shrimp by HPLC |
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| Abstract: |
| A high performance liquid chromatographic method was developed for simultaneous determination of olaquindox(OLA) and methyl-3-quinoxaline-2-carboxylic acid (MQCA) in carp and shrimp. The analytes were extracted with 0.3mol/L hydrochloric acid and cleaned up on a C18 cartridge. The eluate was collected, dried under nitrogen gas, and reconstituted in primary mobile phase solution. OLA and MQCA was separated on a reversed phase Inertsil? ODS-3 C18 column in combination of a gradient elution, MQCA was detected at 320 nm and OLA at 372 nm with a UV detector, with mobile phase of water-acetonitrile-methanol-0.5% formic acid, flow rate of 1.0 mL/min. Quantitation was performed with external standard. The average recoveries of OLA and MQCA in carp muscle were 83.5%～87.7% and 79.6%～87.4%, respectively, when spiked at levels of 20～200μg/kg and 35～200 μg/kg, respectively; while for shrimp muscle were 74.6%～80.9% and 81.0%～86.6%, respectively, when spiked at 15～200 μg/kg and 30～200 μg/kg, respectively. Intra-day relative standard deviations (RSDs, n=5) were 0.51%～4.47% and inter-day RSDs(n=3) were 0.66%～7.58%. The limits of detection (LOD) of OLA and MQCA in fish were 6 μg/kg and 10 μg/kg, respectively, and the limits of quantification (LOQ) were 20 μg/kg and 35 μg/kg respectively; the LODs of the two analytes in shrimp were 4.5 μg/kg and 8 μg/kg and the LOQs were 15 μg/kg and 30 μg/kg, respectively. |
| Key words: Olaquindox Methyl-3-quinoxaline-2-carboxylic acid Residue HPLC Carp Shrimp |
