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高效液相色谱-串联质谱法测定动物源食品中喹乙醇与卡巴氧残留量 | |
其他题名 | Determination of Olaquindox and Carbadox Residues in Animal Originated Food by High Performance Liquid Chromatography -Tandem Mass Spectrometry |
郑玲; 吴玉杰; 赵永锋; 郭蔚; 陈智刚 | |
来源期刊 | 分析测试学报
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ISSN | 1004-4957 |
出版年 | 2014 |
卷号 | 33期号:1页码:21-26 |
中文摘要 | 建立了动物源食品猪肉、鸡肉和鱼肉中喹喔啉类兽药喹乙醇(OLQ)、卡巴氧(CBX)的高效液相色谱-串联质谱测定方法。样品经0. 1 mol/L磷酸二氢钠(pH 6.0)溶液提取,Oasis HLB固相萃取柱净化,流动相定容后,采用Waters Xterra MS C_(18)柱(5 mum,150 mmx2. 1 mm)分离,以乙腈-0. 2%甲酸为流动相进行梯度洗脱,以串联质谱在多反应监测(MRM)正离子模式下检测,基质外标法定量。结果表明,喹乙醇和卡巴氧在质量浓度为1~20 ng/mL 范围内线性关系良好,相关系数为0.998 1 ~ 0. 999 9;各基质在0.2、0.4、2.0 mug/kg 3个加标水平下,喹乙醇和卡巴氧的回收率为70% ~ 93%,相对标准偏差为1.9% ~ 16.7%,定量下限(S/N≥10)均为0.2mug/kg。应用建立的方法对猪肉、鸡肉、鱼肉样品各20个进行检测,并与国标方法进行比较,结果满意。该方法简单、灵敏、稳定,可满足猪肉、鸡肉和鱼肉中喹乙醇、卡巴氧残留的检测与确证需要。 |
英文摘要 | A liquid chromatography -tandem mass spectrometric(LC -MS/MS) method was developed for the simultaneous determination of olaquindox(OLQ) and carbadox(CBX) in animal originated foods (pork, chicken and fish). The CBX and OLQ were extracted with 0. 1 mol/L sodium dihydrogen phosphate (NaH_2PO_4) solution (pH 6. 0) and cleaned up with solid-phase extraction Oasis HLB column. The separation of compounds was carried on a Waters Xterra MS C_(18) column (5 mum, 150 mm *2. 1 mm) by gradient elution using acetonitrile -0. 2% formic acid as mobile phase. The analyte was detected by tandem mass spectrometry under multiple reaction monitoring(MRM) mode with positive electrospray ionization. The CBX and OLQ were quantified by the matrix-matched external standard method. The results showed that the calibration curves of CBX and OLQ were linear in the range of 1 -20 ng/mL with correlation coefficients of 0. 998 1 -0. 999 9. The average recoveries of CBX and OLQ at spiked concentration levels of 0. 2, 0. 4, 2. 0 mug/kg ranged from 70% to 93% with relative standard deviations (RSDs) of 1. 9% -16. 7%. The limits of quantitation (LOQ, S/N ≥10) for two compounds were both 0.2 mug/kg. The established method was used for the determination of real samples(including pork, fish, chicken samples) and the result was compared with that of the national standard method. The result showed that the method was sensitive and accurate, and was suitable for the determination and confirmation of olaquindox and carbadox in pork, chicken and fish samples. |
中文关键词 | 喹乙醇 ; 卡巴氧 ; 液相色谱-串联质谱 ; 动物源食品 |
英文关键词 | olaquindox carbadox LC -MS/MS animal originated food |
语种 | 中文 |
国家 | 中国 |
收录类别 | CSCD |
WOS类目 | CHEMISTRY ANALYTICAL ; PHARMACOLOGY PHARMACY |
WOS研究方向 | Chemistry ; Pharmacology & Pharmacy |
CSCD记录号 | CSCD:5042589 |
资源类型 | 期刊论文 |
条目标识符 | http://119.78.100.177/qdio/handle/2XILL650/231032 |
作者单位 | 广西出入境检验检疫局, 南宁, 广西 530021, 中国 |
推荐引用方式 GB/T 7714 | 郑玲,吴玉杰,赵永锋,等. 高效液相色谱-串联质谱法测定动物源食品中喹乙醇与卡巴氧残留量[J],2014,33(1):21-26. |
APA | 郑玲,吴玉杰,赵永锋,郭蔚,&陈智刚.(2014).高效液相色谱-串联质谱法测定动物源食品中喹乙醇与卡巴氧残留量.分析测试学报,33(1),21-26. |
MLA | 郑玲,et al."高效液相色谱-串联质谱法测定动物源食品中喹乙醇与卡巴氧残留量".分析测试学报 33.1(2014):21-26. |
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