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Application of high-performance liquid chromatography–UV detection to quantification of clenbuterol in bovine liver samples

机译:高效液相色谱-紫外检测在牛肝样品中盐酸克伦特罗定量中的应用

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Abstract A method for the determination of clenbuterol (CLB) concentration in bovine liver by reversed-phase high-performance liquid chromatography (HPLC) with {UV} detection was developed. The sample was extracted with acetonitrile and isopropanol, followed by {HPLC} analysis. A reverse-phase column {C18} was used, with a {UV} detector at 214?nm and 0.05?M NaH2PO4 (pH 3.0)/acetonitrile (85:15, v/v) as the mobile phase. The accuracy of the analytical method was estimated by spiking bovine liver samples with three different concentrations of {CLB} (5.24?ng/g, 20.98?ng/g, and 41.96?ng/g) and recovery of 111.7%, 82.0%, and 84.8%, respectively, was obtained. The precision of the method was estimated by the relative standard deviation, which was??4.74%. The limit of detection and quantification of {CLB} were 0.20?ng/g and 0.42?ng/g of liver sample, respectively, and the retention time was 24.82 minutes. The recent discovery of {CLB} contamination in Mexican food led to the specific inspection of a distribution center for this β-agonist, involving the analysis of a total of 78 bovine liver samples. Of all samples screened, 62% of them had concentrations above the maximum residue limit of 0.6?ng/g set by the United Nations Food and Agricultural Organization for CLB. The analytical method was found to be rapid, sensitive, accurate, repeatable, and reproducible, and could be applied to the measurement of {CLB} concentration in bovine liver.
机译:摘要建立了一种用 UV检测反相高效液相色谱法测定牛肝中盐酸克伦特罗的方法。用乙腈和异丙醇萃取样品,然后进行HPLC分析。使用反相柱 {C18 },在214?nm处用 {UV }检测器和0.05?M NaH2PO4(pH 3.0)/乙腈(85:15,v / v)作为流动相。通过用三种不同浓度的 {CLB }(5.24?ng / g,20.98?ng / g和41.96?ng / g)加标牛肝样品并回收率111.7%,82.0评估分析方法的准确性。分别获得%和84.8%。该方法的精度由相对标准偏差估计,该相对标准偏差为α<4.74%。 {CLB }的肝样品检出限和定量限分别为0.20?ng / g和0.42?ng / g,保留时间为24.82分钟。最近在墨西哥食品中发现 {CLB }污染,导致对该β激动剂的配送中心进行了专门检查,涉及对总共78个牛肝样品的分析。在所有筛选出的样品中,有62%的浓度超过了联合国粮食及农业组织(CLB)设定的最大残留限量0.6ng / g。该分析方法是快速,灵敏,准确,可重复和可重复的,可用于牛肝中 {CLB }浓度的测量。

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