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Development and validation of a high performance liquid chromatography/diode array detection method for estrogen determination: Application to residual analysis in meat products
Open Chemistry ( IF 2.1 ) Pub Date : 2020-08-07 , DOI: 10.1515/chem-2020-0118
Sadeem S. Alqahtani 1 , Deema M. Bin Humaid 1 , Sabreen H. Alshail 1 , Dalal T. AlShammari 1 , Hessa Al-Showiman 1 , Nourah Z. Alzoman 1 , Hadir M. Maher 1, 2
Affiliation  

Abstract In this work, an HPLC-DAD method was developed for the residual analysis of some estrogens such as estrone (E1), 17-β estradiol (E2), estriol (E3), natural estrogens, and 17-α ethinylestradiol (E4), an exoestrogen, in meat samples of different categories (chicken, n = 155, beef, n = 124, sheep, n = 122, and camels, n = 40), collected from the Saudi Market. Although banned, the use of E4 as a growth promoter in the black market is still encountered. Symmetry C18 column (3.5 µm, 4.6 mm × 150 mm) was used with a mobile phase consisting of 50% aqueous acetonitrile. Protein precipitation with acetonitrile was used for the sample preparation. The method was fully validated, as per the ICH guidelines, in the concentration ranges of 0.35–125 µg/g (E1, E2), 0.188–125 µg/g (E3), and 0.188–450 µg/g (E4). The method allowed the trace analysis of estrogens with LOD values of 0.094 (E3, E4) and 0.126 µg/g (E1, E2), and LOQ values of 0.188 (E3, E4) and 0.350 µg/g (E1, E2). The analyzed samples contained different levels of estrogens. Within the same category, processed products contained the highest levels of E4, while the internal organs contained the least estrogen content. Finally, the estimated daily intake, µg/kg bw/day, of estrogens through the consumption of meat-based food products was calculated.

中文翻译:

雌激素测定的高效液相色谱/二极管阵列检测方法的开发和验证:在肉制品残留分析中的应用

摘要 本工作建立了一种 HPLC-DAD 方法,用于分析雌酮 (E1)、17-β 雌二醇 (E2)、雌三醇 (E3)、天然雌激素和 17-α 炔雌醇 (E4) 等雌激素的残留。 ,一种外雌激素,在不同类别的肉类样品中(鸡肉,n = 155,牛肉,n = 124,绵羊,n = 122,骆驼,n = 40),从沙特市场收集。虽然被禁止,但仍会遇到在黑市中使用 E4 作为生长促进剂的情况。Symmetry C18 色谱柱(3.5 µm,4.6 mm × 150 mm)使用由 50% 乙腈水溶液组成的流动相。用乙腈沉淀蛋白质用于样品制备。根据 ICH 指南,该方法在 0.35–125 µg/g (E1, E2)、0.188–125 µg/g (E3) 和 0.188–450 µg/g (E4) 的浓度范围内得到了充分验证。该方法允许对 LOD 值为 0.094 (E3, E4) 和 0.126 µg/g (E1, E2),LOQ 值为 0.188 (E3, E4) 和 0.350 µg/g (E1, E2) 的雌激素进行痕量分析。分析的样品含有不同水平的雌激素。在同一类别中,加工产品的 E4 含量最高,而内脏的雌激素含量最低。最后,计算了通过食用肉类食品估计的雌激素每日摄入量(微克/千克体重/天)。
更新日期:2020-08-07
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