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采用聚(乙烯基咪唑-共-乙二醇二甲基丙烯酸酯)整体毛细管液相色谱法,用紫外检测法同时测定蔬菜中的硝酸盐和亚硝酸盐。

Simultaneous determination of nitrate and nitrite in vegetables by poly(vinylimidazole-co-ethylene dimethacrylate) monolithic capillary liquid chromatography with UV detection.

机构信息

Department of Chemistry, Soochow University, 70 Linhsi Road, Shihlin, 11102, Taipei, Taiwan.

Department of Chemistry, Soochow University, 70 Linhsi Road, Shihlin, 11102, Taipei, Taiwan.

出版信息

Talanta. 2019 Dec 1;205:120082. doi: 10.1016/j.talanta.2019.06.082. Epub 2019 Jun 22.

Abstract

Simultaneous determination of nitrate (NO) and nitrite (NO) in vegetables was performed on a poly(1-vinylimidazole-co-ethylene dimethacrylate) (VIM-EDMA) monolithic column by capillary liquid chromatography (LC) with UV detection. Good linearity (0.5-100 μg mL i.e. 12.5 -2500 μg g in vegetables) was obtained with coefficient of determination > 0.996. Limits of detection (signal-to-noise ratio: S/N= 3) were estimated at 0.06 and 0.05 μg mL, which corresponded to 1.50 and 1.25 μg g for NO and NO, respectively, in vegetables. The limits of quantification (S/N= 10) were estimated at 0.17 and 0.16 μg mL (4.25 and 4.00 μg g in vegetables) for NO and NO, respectively. Although the detection limits were relatively higher than other LC-UV techniques, this proposed method offered satisfactory sensitivity for complying the Acceptable Daily Intake (ADI) levels set by EU to monitor the occurrence of NO and NOin vegetables. The intra-day/inter-day precision (0.14-3.35%/0.06-6.93%) and accuracy (90.33-103.32%/96.00-101.26%) were also examined for method validation. No obvious carry-over and decline of separation efficiency were observed for more than 200 analyses of real samples. The occurrence of NO and NOin various vegetable samples was investigated to demonstrate the potential of utilizing the developed polymeric monolith-based capillary LC-UV method for food safety application.

摘要

采用聚(1-乙烯基咪唑-共-乙二醇二甲基丙烯酸酯)(VIM-EDMA)整体柱毛细管液相色谱(LC)-紫外检测法同时测定蔬菜中的硝酸盐(NO)和亚硝酸盐(NO)。在蔬菜中,线性范围为 0.5-100μg mL (即 12.5-2500μg g),相关系数大于 0.996。检测限(信噪比:S/N=3)估计为 0.06 和 0.05μg mL,相当于蔬菜中 NO 和 NO 的检出限分别为 1.50 和 1.25μg g。定量限(S/N=10)估计为 0.17 和 0.16μg mL,相当于蔬菜中 NO 和 NO 的定量限分别为 4.25 和 4.00μg g。尽管检测限相对高于其他 LC-UV 技术,但该方法提供了令人满意的灵敏度,符合欧盟设定的可接受日摄入量(ADI)水平,以监测蔬菜中 NO 和 NO 的发生。日内/日间精密度(0.14-3.35%/0.06-6.93%)和准确度(90.33-103.32%/96.00-101.26%)也进行了方法验证。对于超过 200 次实际样品分析,未观察到明显的峰间拖尾和分离效率下降。研究了各种蔬菜样品中 NO 和 NO 的发生情况,以证明开发的基于聚合物整体柱的毛细管 LC-UV 方法在食品安全应用中的潜力。

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