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分光荧光光度法测定食品样品中残留硝西泮的含量。

Spectrofluorometric determination of residual amounts of nitroxynil in food samples.

机构信息

Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Mansoura University, Mansoura, 35516, Egypt.

Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Mansoura University, Mansoura, 35516, Egypt; Pharmaceutical Chemistry Department, Faculty of Pharmacy, Horus University- Egypt, New Damietta, 34518, Egypt.

出版信息

Spectrochim Acta A Mol Biomol Spectrosc. 2022 Jun 5;274:120993. doi: 10.1016/j.saa.2022.120993. Epub 2022 Feb 5.

Abstract

Because of the frequent treatment of dairy cows with nitroxynil (NTX), the presence of the later residues in animal tissues and milk has a significant concern. The quantum yield of the reaction product was calculated. A highly sensitive and rapid spectrofluorometric method for determining the anthelmintic drug (NTX) residual amounts is developed. The proposed approach is based on using Zn/HCl to reduce NTX nitro group to an amino group, resulting in a highly fluorescent derivative that was detected at each of λ 302 nm and 364 nm after excitation at λ = 277 nm. The experimental conditions were carefully studied and optimized. The proposed approach showed good linearity (r ≥ 0.9998) with linearity range of 10.0-100.0 ng/mL with a detection limit of 1.89 ng/mL, 1.27 ng/mL and quantification limit of 5.73 ng/mL, 3.86 ng/mL at λ 302 nm and 364 nm, respectively; that is far below the Minimum Regulatory Limits (MRLs) of NTX in animal tissues and milk. The proposed approach was successfully applied for the analysis of the drug in its veterinary formulations, and the obtained results agreed well with those of the official British Pharmacopeia method. Moreover, the proposed method's application was extended to efficiently determine the residues of nitroxynil in meat, liver, kidney and milk samples.

摘要

由于奶牛经常接受硝羟吡啶(NTX)治疗,因此动物组织和牛奶中存在的该药物残留令人高度关注。计算了反应产物的量子产率。建立了一种用于检测驱虫药(NTX)残留量的高灵敏度和快速荧光分光光度法。该方法基于使用 Zn/HCl 将 NTX 的硝基还原为氨基,生成一种高度荧光的衍生物,在 277nm 激发下,在 λ 302nm 和 364nm 处分别检测到该衍生物。仔细研究并优化了实验条件。该方法在 λ 302nm 和 364nm 处分别在 10.0-100.0ng/mL 范围内具有良好的线性关系(r≥0.9998),检测限为 1.89ng/mL、1.27ng/mL,定量限为 5.73ng/mL、3.86ng/mL;这远低于动物组织和牛奶中 NTX 的最低监管限量(MRLs)。该方法成功地应用于兽医制剂中药物的分析,并且获得的结果与英国药典官方方法的结果吻合良好。此外,该方法还被扩展用于有效地检测肉类、肝脏、肾脏和牛奶样品中硝羟吡啶的残留。

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