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  • 食品科学与工程领域高质量科技期刊分级目录第一方阵T1
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中国精品科技期刊2020
王京, 叶佳明, 钟世欢, 王潇, 陈青俊. 超高效液相色谱-四极杆飞行时间质谱法快速测定畜禽产品中抗组胺类药物残留[J]. 食品工业科技, 2021, 42(5): 250-256,264. DOI: 10.13386/j.issn1002-0306.2020050044
引用本文: 王京, 叶佳明, 钟世欢, 王潇, 陈青俊. 超高效液相色谱-四极杆飞行时间质谱法快速测定畜禽产品中抗组胺类药物残留[J]. 食品工业科技, 2021, 42(5): 250-256,264. DOI: 10.13386/j.issn1002-0306.2020050044
WANG Jing, YE Jiaming, ZHONG Shihuan, WANG Xiao, CHEN Qingjun. Determination of Antihistamine Residues in Livestock and Poultry Products by Ultra Performance Liquid Chromatography-Quadrupole-Time of Flight Mass Spectrometry[J]. Science and Technology of Food Industry, 2021, 42(5): 250-256,264. DOI: 10.13386/j.issn1002-0306.2020050044
Citation: WANG Jing, YE Jiaming, ZHONG Shihuan, WANG Xiao, CHEN Qingjun. Determination of Antihistamine Residues in Livestock and Poultry Products by Ultra Performance Liquid Chromatography-Quadrupole-Time of Flight Mass Spectrometry[J]. Science and Technology of Food Industry, 2021, 42(5): 250-256,264. DOI: 10.13386/j.issn1002-0306.2020050044

超高效液相色谱-四极杆飞行时间质谱法快速测定畜禽产品中抗组胺类药物残留

Determination of Antihistamine Residues in Livestock and Poultry Products by Ultra Performance Liquid Chromatography-Quadrupole-Time of Flight Mass Spectrometry

  • 摘要: 建立超高效液相色谱-四极杆飞行时间质谱(UPLC-Q-TOF/MS)快速测定畜禽产品中19种抗组胺类药物及代谢物残留的方法。样品用乙腈-乙酸乙酯溶液提取,提取液经增强型脂质去除剂(EMR)结合经氧化修饰的多壁碳纳米管(MWCNTs)净化,以0.1%甲酸水-0.1%甲酸乙腈作为流动相进行梯度洗脱,在EclipsePlus-C18(50 mm×2.1 mm,1.8 μm)色谱柱上分离,柱温40℃,流速0.3 mL/min,进样量5 μL,Q-TOF/MS电喷雾正离子模式分析检测。在全扫描模式下采集一级质谱数据,以待测物的准分子离子峰的峰面积定量,以保留时间、精确质量数、同位素丰度比等特征信息定性。在Target MS/MS模式下靶向采集二级质谱数据,通过特征碎片离子的精确质量数等信息进一步确证。结果表明,所有药物在浓度范围内线性良好,决定系数均大于0.996,不同阴性样品基质中(牛肉、鸡肉、猪肝)在3个浓度水平加标试验回收率在78.2%~105.3%之间,相对标准偏差(RSD)为3.2%~8.2%,方法检出限(LOD,S/N≥3)为0.5~2.0 μg/kg,定量限为1.5~6.0 μg/kg。本方法简便快速,灵敏度高,选择性好,结果准确,适用于畜禽产品中19种抗组胺类药物及代谢物的快速筛查和定量测定。

     

    Abstract: A rapid method for the determination of 19 antihistamines and metabolites residues in livestock and poultry products by UPLC-Q-TOF/MS was developed. Samples,were extracted with acetonitrile-ethyl acetate solution extract by enhanced matrix removal(EMR)combined with oxidative modification of multi-walled carbon nanotubes(MWCNTs)purification,with 0.1% formic acid formic acid water-0.1% acetonitrile as mobile phase in gradient elution,in EclipsePlus-C18(50 mm×2.1 mm,1.8 μm)on the chromatographic column separation,column temperature 40 ℃,the flow rate of 0.3 mL/min,sample quantity was 5 μL,Q-TOF/MS electrospray cations pattern analysis. The first-order mass spectrometry data were collected in the full-scan mode to quantify the peak area of the excimer ion peak of the measured object,and to determine the quality of the characteristic information such as retention time,accurate mass number and isotope abundance ratio. In the Target MS/MS mode,the secondary mass spectrometry data were targeted and further confirmed by the accurate mass number of the characteristic fragment ions. Statistics indicated that this method whose RSD was 3.2%~8.2%,had a good linear with R2>0.996 in their ranges of linearity,what’s more,the LODs of which were 0.5~2.0 μg/kg and the LOQs were 1.5~6.0 μg/kg along with a hige recovery rate ranged 78.2%~105.3% from different sample matrixes(beef,chicken,pork liver)added 3 levels of concentration.. This method is simple,rapid,sensitive,selective and accurate,and is suitable for rapid screening and quantitative determination of 19 antihistamines and metabolites in livestock and poultry products.

     

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