首页> 外文期刊>Journal of chromatography, B. Analytical technologies in the biomedical and life sciences >Determination of gamithromycin residues in eggs, milk and edible tissue of food-producing animals by solid phase extraction combined with ultrahigh-performance liquid chromatography-tandem mass spectrometry
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Determination of gamithromycin residues in eggs, milk and edible tissue of food-producing animals by solid phase extraction combined with ultrahigh-performance liquid chromatography-tandem mass spectrometry

机译:用固相萃取结合超高效液相色谱 - 串联质谱法测定食品生产动物的鸡蛋,牛奶和食用动组织中的鸡蛋,牛奶和可食用组织中的测定

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摘要

A high throughput method was developed and validated for the quantitation of gamithromycin residues in eggs, milk and animal tissues (leg muscle, kidney, liver and fat) of different species and genera. This was undertaken using ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The samples were extracted with acetonitrile and purified using an Oasis MCX solid phase extraction cartridge. Subsequently, a C18 column was used for chromatographic separation using acetonitrile and 0.1% formic acid as the mobile phase. LC-MS/MS in positive ESI and multiple reaction monitoring mode with gamithromycin-D4 as the internal standard was used for detection and quantification of gamithromycin. The method was successfully calibrated in the range of 1.0?200 ?g/kg. The limit of detection (LOD) and limit of quantification (LOQ) for gamithromycin was 0.30?0.40 ?g/kg and 0.80 ? 1.0 ?g/kg, respectively. The average recoveries of the analyte fortified at three levels ranged from 84.2% to 115.9%, with a relative standard deviation <10%. The proposed method has been successfully used to monitor real samples, and shown to be sensitive, rapid, and convenient. Hence, this method could be used for regulatory purposes to screen for the presence of gamithromycin residues in eggs, milk and target tissues.
机译:建立并验证了一种高通量方法,用于测定鸡蛋、牛奶和不同物种和属的动物组织(腿部肌肉、肾脏、肝脏和脂肪)中的伽马霉素残留量。这是通过超高效液相色谱-串联质谱(UHPLC-MS/MS)进行的。样品用乙腈萃取,并用Oasis MCX固相萃取柱纯化。随后,使用C18柱,以乙腈和0.1%甲酸为流动相进行色谱分离。采用LC-MS/MS,在ESI阳性和多反应监测模式下,以gamithromycin-D4为内标检测和定量gamithromycin。该方法在1.0?的范围内成功校准?200 ?g/kg。gamithromycin的检测限(LOD)和定量限(LOQ)为0.30?0.40 ?g/kg和0.80?1.0 ?g/kg。在三个水平强化的分析物的平均回收率在84.2%到115.9%之间,相对标准偏差<10%。该方法已成功应用于实际样品的监测,具有灵敏、快速、方便的特点。因此,该方法可用于监管目的,以筛查鸡蛋、牛奶和靶组织中是否存在伽红霉素残留。

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