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高效液相色谱法测定大蒜鳞茎中马来酰肼残留量。

Determination of maleic hydrazide residues in garlic bulbs by HPLC.

机构信息

Laboratory of Environmental Toxicology-IMBECU. CONICET, CCT-Mendoza. Av. Ruiz Leal s/n, Parque General San Martín, CC. 131, M 5500 IRA, Mendoza, Argentina.

出版信息

Talanta. 2012 Jan 30;89:369-76. doi: 10.1016/j.talanta.2011.12.045. Epub 2011 Dec 22.

Abstract

In recent years, the release of information about the preventative and curative properties of garlic on different diseases and their benefits to human health has led to an increase in the consumption of garlic. To meet the requirements of international markets and reach competitiveness and profitability, farmers seek to extend the offer period of fresh garlic by increasing post-harvest life. As a result, the use of maleic hydrazide (1,2-dihydropyridazine-3,6-dione) [MH], a plant growth regulator, has been widespread in various garlic growing regions of the world. The present work was undertaken to develop and validate a new analytical procedure based on MH extraction from garlic previously frozen by liquid nitrogen and submitted to low temperature clean-up. The applicability of the method by analysis of garlic samples from a commercial plantation was also demonstrated. The influence of certain factors on the performance of the analytical methodology were studied and optimized. The approach is an efficient extraction, clean-up and determination alternative for MH residue-quantification due to its specificity and sensitivity. The use of liquid nitrogen during the sample preparation prevents the degradation of the analyte due to oxidation reactions, a major limiting factor. Moreover, the method provides good linearity (r(2): 0.999), good intermediate precision (coefficient of variation (CV): 8.39%), and extracts were not affected by the matrix effect. Under optimized conditions, the limit of detection (LOD) (0.33 mg kg(-1)) was well below the maximum residue level (MRL) set internationally for garlic (15 mg kg(-1)), with excellent rates of recovery (over 95%), good repeatability and acceptable accuracy (CV averaged 5.74%), since garlic is a complex matrix. The analytical performance of the methodology presented was compared with other techniques already reported, with highly satisfactory results, lower LOD and higher recoveries rates. In addition, the extraction process is simple, not expensive, easily executable and requires lower volumes of organic solvent. The proposed methodology removes the need of extensive typical laboratory extraction procedures, reducing the amount of time needed for pesticide analysis and increasing sample throughput. Adopting this method gives food safety laboratories the potential to increase cost savings by a suitable technique in routine testing to determine MH residues in garlic.

摘要

近年来,大蒜在预防和治疗各种疾病方面的功效及其对人类健康的益处的信息不断被公布,导致大蒜的消费不断增加。为了满足国际市场的要求,提高竞争力和盈利能力,农民们寻求通过延长新鲜大蒜的供应期来增加收获后的寿命。因此,在世界上各种大蒜种植区,普遍使用了马来酰肼(1,2-二氢哒嗪-3,6-二酮)[MH],一种植物生长调节剂。本工作旨在开发和验证一种新的分析方法,该方法基于 MH 从液氮预冷冻的大蒜中提取,并进行低温净化。还通过对商业种植园中大蒜样品的分析证明了该方法的适用性。研究并优化了某些因素对分析方法性能的影响。该方法是一种高效的提取、净化和测定 MH 残留量的替代方法,具有特异性和灵敏度。在样品制备过程中使用液氮可以防止由于氧化反应而导致分析物降解,这是一个主要的限制因素。此外,该方法提供了良好的线性(r²:0.999)、良好的中间精密度(变异系数(CV):8.39%),并且提取物不受基质效应的影响。在优化条件下,检测限(LOD)(0.33mgkg-1)远低于国际上设定的大蒜最大残留限量(MRL)(15mgkg-1),回收率非常高(超过 95%),重复性好,准确性可接受(平均 CV 为 5.74%),因为大蒜是一种复杂的基质。所提出的方法的分析性能与其他已报道的技术进行了比较,结果非常令人满意,LOD 更低,回收率更高。此外,提取过程简单、不昂贵、易于执行,并且需要的有机溶剂体积较小。该方法不需要广泛的典型实验室提取程序,减少了农药分析所需的时间,并增加了样品通量。采用这种方法,食品安全实验室可以通过在常规检测中采用合适的技术来确定大蒜中的 MH 残留量,从而有潜力节省成本。

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