Universidade Federal de Santa Catarina (UFSC), Departamento de Química, Programa de Pós-graduação em Química, Florianópolis, SC, Brazil; Ministério da Agricultura, Pecuária e Abastecimento (MAPA), Laboratório Federal de Defesa Agropecuária, Seção Laboratorial Avançada, São José, SC, Brazil; Instituto Catarinense de Sanidade Agropecuária, Florianópolis, SC, Brazil.
Ministério da Agricultura, Pecuária e Abastecimento (MAPA), Laboratório Federal de Defesa Agropecuária, Seção Laboratorial Avançada, São José, SC, Brazil; Instituto Catarinense de Sanidade Agropecuária, Florianópolis, SC, Brazil.
Food Res Int. 2022 Nov;161:111780. doi: 10.1016/j.foodres.2022.111780. Epub 2022 Aug 23.
Sulfite is widely used to prevent enzymatic browning in shrimp and lobster processing. However, sulfite may cause allergy in sensitive consumers. Thus, regulatory agencies set limits for its use. Sulfite is usually controlled by the normalized Monier-Williams (MW) titrimetric method that allows a limited number of samples to be analyzed. This manuscript consolidates an innovative method for sulfite inspection in seafood by capillary zone electrophoresis with diode array detector (CZE-DAD). A simple, fast, and simultaneous extraction and derivatization method was developed to provide high throughput for analytical routine. The high instability of the sulfite was suppressed by its derivatization with formaldehyde producing hydroxymethylsulfonate. The evaluation of its analytical performance yielded excellent results in compliance with the strict parameters required for metrological accreditation. The CZE-DAD method was selective and specific when submitted to confirmatory evaluations by liquid chromatography coupled to mass spectrometry. The limit of detection (3.50 mg kg), limit of quantitation (11.7 mg kg) and recoveries (99-103%) were adequate for sample analysis. The measurement uncertainty was estimated by the propagation of errors and experimental standard uncertainties (precision, accuracy, and analytical curves) and type B uncertainties from traceable measurement instruments. The low relative uncertainty (10%) and the adequate reproducibility demonstrated method suitability. The CZE-DAD results were compared to the MW method through the respective expanded standard uncertainties and normalized error. This new method is promising to be used in seafood inspection and continuous laboratory evaluations using instrumentation not very expensive to acquire and maintain.
亚硫酸盐被广泛用于防止虾和龙虾加工过程中的酶促褐变。然而，亚硫酸盐可能会引起敏感消费者的过敏反应。因此，监管机构对其使用设定了限制。亚硫酸盐通常通过归一化的 Monier-Williams（MW）滴定法进行控制，该方法允许分析有限数量的样品。本文通过带有二极管阵列检测器的毛细管区带电泳（CZE-DAD）整合了一种用于海鲜中亚硫酸盐检测的创新方法。开发了一种简单、快速且同时进行提取和衍生化的方法，为分析常规提供高通量。通过将亚硫酸盐与甲醛衍生化生成羟甲基磺酸盐来抑制其高不稳定性。对其分析性能的评估结果符合计量认证要求的严格参数，得出了极好的结果。当通过与质谱联用的液相色谱进行确证评估时，CZE-DAD 方法具有选择性和特异性。检测限（3.50 mg kg）、定量限（11.7 mg kg）和回收率（99-103%）足以进行样品分析。通过误差传播和实验标准不确定度（精密度、准确度和分析曲线）以及可溯源测量仪器的 B 类不确定度来估计测量不确定度。相对不确定度低（10%）且重现性良好，证明了方法的适用性。通过各自的扩展标准不确定度和归一化误差将 CZE-DAD 结果与 MW 方法进行了比较。该新方法有望用于海鲜检测和使用购置和维护成本不高的仪器进行连续实验室评估。
