Center for Food Safety and Applied Nutrition, U.S. Food and Drug Administration, College Park, Maryland, USA.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2020 May;37(5):723-730. doi: 10.1080/19440049.2020.1727965. Epub 2020 Mar 11.
In the US, sulphites must be declared on the label if they are present in concentrations greater than 10 mg/kg (determined as) SO because an allergic-like response has been reported in a small subset of the population upon consumption of sulphite-containing products. The most widely used method for sulphite determination, the optimised Monier-Williams (OMW), produces false positive results with vegetables from the (garlic) and (cabbage) genera due to extraction conditions that are thought to cause endogenous sulphur compounds to release SO. Recently, an LC-MS/MS method was developed for sulphites but has only been tested with samples that are 100% or . Since regulatory samples may contain these vegetables as ingredients, additional investigations were necessary to determine the potential extent of false positives. Four blank matrices, chips, phyllo shells, hummus, and quinoa were spiked with various concentrations of onion and garlic powders. The sulphite concentrations were determined using an LC-MS/MS method. The matrix is extracted with a buffered formaldehyde solution, converting free and reversibly bound sulphite to the stable formaldehyde adduct, hydroxymethylsulfonate (HMS). It was determined that even at concentrations up to 8% garlic powder or 2% onion powder, the measured sulphite concentration was below the 10 mg/kg SO labelling threshold. Commercial dried garlic powders were evaluated to determine the variation in responses that might be encountered in future regulatory samples. Recovery studies were conducted to determine if these methods would detect added sulphite. The ability to eliminate false positives due to these ingredients will result in a greater reliability in the accurate determination of added sulphite to ensure compliance with labelling requirements.
在美国,如果亚硫酸盐浓度大于 10mg/kg(以 SO 计),则必须在标签上注明,因为有报道称一小部分人群在食用含亚硫酸盐的产品后会出现类似过敏的反应。最广泛使用的亚硫酸盐测定方法,即优化的 Monier-Williams(OMW)法,由于提取条件会导致内源性硫化合物释放 SO,因此会对来自大蒜属和甘蓝属的蔬菜产生假阳性结果。最近,开发了一种用于亚硫酸盐的 LC-MS/MS 方法,但仅在 100%洋葱或大蒜的样品上进行了测试。由于监管样品可能含有这些蔬菜作为成分,因此需要进行额外的调查以确定假阳性的潜在程度。四个空白基质(芯片、千层酥壳、鹰嘴豆泥和藜麦)用各种浓度的洋葱和大蒜粉进行了加标。使用 LC-MS/MS 方法测定亚硫酸盐浓度。基质用缓冲甲醛溶液提取,将游离和可逆结合的亚硫酸盐转化为稳定的甲醛加合物羟甲基磺酸盐(HMS)。结果表明,即使添加高达 8%的大蒜粉或 2%的洋葱粉,测得的亚硫酸盐浓度仍低于 10mg/kg SO 的标签阈值。对商业干大蒜粉进行了评估,以确定在未来的监管样品中可能遇到的响应变化。进行了回收率研究,以确定这些方法是否能检测到添加的亚硫酸盐。消除这些成分造成的假阳性的能力将使准确测定添加亚硫酸盐的可靠性更高,从而确保符合标签要求。