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Development of an analytical method for multi-residue quantification of 18 anthelmintics in various animal-based food products using liquid chromatography-tandem mass spectrometry

机译:使用液相色谱 - 串联质谱法在各种动物型食品中18个触发仪的多残基定量分析方法的研制

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In this study, we developed a simple screening procedure for the determination of 18 anthelmintics (including benzimidazoles, macrocyclic lactones, salicylanilides, substituted phenols, tetrahydropyrimidines, and imidazothiazoles) in five animal-derived food matrices (chicken muscle, pork, beef, milk, and egg) using liquid chromatography-tandem mass spectrometry. Analytes were extracted using acetonitrile/1% acetic acid (milk and egg) and acetonitrile/1% acetic acid with 0.5?mL of distilled water (chicken muscle, pork, and beef), and purified using saturatedn-hexane/acetonitrile. A reversed-phase analytical column and a mobile phase consisting of (A) 10?mM ammonium formate in distilled water and (B) methanol were used to achieve optimal chromatographic separation. Matrix-matched standard calibration curves (R2≥0.9752) were obtained for concentration equivalent to?×1/2,?×1,?×2,?×3,?×4, and?×5 fold the maximum residue limit (MRL) stipulated by the Korean Ministry of Food and Drug Safety. Recoveries of 61.2–118.4%, with relative standard deviations (RSDs) of ≤19.9% (intraday and interday), were obtained for each sample at three spiking concentrations (×1/2,?×1, and?×2 the MRL values). Limits of detection, limits of quantification, and matrix effects were 0.02–5.5?μg/kg, 0.06–10?μg/kg, and??98.8 to 13.9% (at 20?μg/kg), respectively. In five samples of each food matrix (chicken muscle, pork, beef, milk, and egg) purchased from large retailers in Seoul that were tested, none of the target analytes were detected. It has therefore been shown that this protocol is adaptable, accurate, and precise for the quantification of anthelmintic residues in foods of animal origin.
机译:在这项研究中,我们开发了一种简单的筛选程序,用于测定18例,包括苯并咪唑,丙酰胺内酯,水杨酰胺,取代的酚,四氢吡啶胺和咪唑基唑(鸡肉,猪肉,牛肉,牛奶,和蛋)使用液相色谱 - 串联质谱法。使用乙腈/ 1%乙酸(牛奶和鸡蛋)和乙腈/ 1%乙酸用0.5?ml蒸馏水(鸡肉肌肉,猪肉和牛肉)来提取分析物,并使用饱和己烷/乙腈纯化。反相分析柱和由蒸馏水中的(a)10?mm甲酸铵组成的流动相,用于达到最佳的色谱分离。获得矩阵匹配的标准校准曲线(R2≥0.9752)获得浓度等效于Δ×1/2,×1,×2,×3,×4,×5折叠最大残留限制(MRL )由韩国食品和药物安全部规定。在三个尖峰浓度(×1/2,×1,和α2的每个样品中,每个样品获得61.2-118.4%的61.2-118.4%(Corladay和第二个)(盘中和间期),获得每个样品)。检测限,定量限值和基质效应分别为0.02-5.5Ωμg/ kg,0.06-10Ωμg/ kg,分别为98.8至13.9%(以20μg/ kg)。在从大型零售商购买的每种食物基质(鸡肉肌肉,猪肉,牛奶,牛奶和鸡蛋)的五个样本中被测试的,没有检测到任何靶分析物。因此,已经表明该方案适应性,准确,精确,精确地用于在动物来源食品中定量扁平症残留物。

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