蜜胺餐具中三聚氰胺单体的迁移规律研究

结合蜜胺餐具的实际使用情况,选用合适的食品模拟物进行迁移实验,采用LC-MS/MS法测定三聚氰胺迁移量,研究蜜胺餐具中三聚氰胺单体的迁移规律。重点考察了食品模拟物种类、接触时间、接触温度、乙酸浓度、乙醇浓度、重复使用和微波加热等迁移条件下蜜胺餐具中三聚氰胺迁移量的变化情况。结果表明酸性食品和牛奶中的三聚氰胺迁移风险较高,且需控制蜜胺餐具的使用温度、盛放时间、重复使用次数及微波加热功率和时间以降低密胺餐具中三聚氰胺迁移风险。      

密胺餐具中三聚氰胺迁移量影响因素分析

目的 对密胺餐具中三聚氰胺迁移量影响因素进行分析。方法 以水、4%乙酸、50%乙醇3种溶剂为浸泡液, 在不同温度下浸泡不同时间, 其浸泡液过滤并用高效液相色谱-质谱法测定, 外标法定量。结果 密胺餐具中三聚氰胺的迁移量和迁移时间、迁移温度、迁移浸泡液相关。三聚氰胺的迁移量随着迁移时间增加、迁移温度升高而升高, 且在酸性模拟溶液中三聚氰胺的迁移量最大。浸泡液为4%乙酸时, 在100 ℃下浸泡1 h时, 三聚氰胺迁移量达到最大值, 密胺碗、饭勺、筷子的迁移量分别为1.94、1.35、1.61 mg/kg。结论 密胺餐具中的三聚氰胺在高温、酸性条件下易迁移, 建议消费者在使用过程中尽量避免在高温、酸性条件下使用, 选择大品牌的厂家生产的有QS标示的产品。     

脲醛树脂制品中甲醛在食品模拟物中迁移的规律

采用乙酰丙酮分光光度法测定脲醛树脂制品在不同类别食品模拟物中、不同使用条件下甲醛的迁移量,并得出其迁移规律:在相同的使用时间和温度下,酸性模拟物中甲醛的迁移量最大;在同种食品模拟物中,甲醛迁移量随着接触时间的延长、接触温度的升高而增加;甲醛迁移量随着使用次数的增加而增加,制品表面磨损后,甲醛的迁移量会迅速增加;脲醛树脂制品在微波条件下使用时,其表面易磨损,且甲醛的迁移量比常规条件下大.     

密胺餐具的鉴别及其三聚氰胺和甲醛迁移风险调查

目的对密胺餐具中三聚氰胺和甲醛迁移量进行调查研究,并对数据进行分析。方法在上海的企业和消费市场采集密胺餐具共40份,采用红外光谱法进行材料鉴别,依照GB 4806.7—2016《食品安全国家标准食品接触用塑料材料及制品》和GB 31604.1—2015《食品安全国家标准食品接触材料及制品迁移试验通则》进行迁移试验,测定三聚氰胺和甲醛迁移量。结果密胺餐具存在材质未标识、标识不清或标识有误的现象;脲醛树脂中三聚氰胺和甲醛的迁移量均高于密胺树脂,且迁出量与温度呈正相关。结论脲醛树脂应用于餐具存在风险,国家标准中有必要增加密胺材质鉴定检测方法。     

竹纤维密胺餐具中三聚氰胺和甲醛在酸性条件下的迁移量测定

目的 通过研究竹纤维密胺餐具中三聚氰胺和甲醛在酸性条件下的迁移规律,讨论影响迁移水平和安全风险的主要因素,对该类产品的安全管理提供建议。方法 采集市场上不同品牌且明确标识含有竹纤维的密胺餐具14种（包括婴幼儿餐具）,选择10%(V/V)乙醇和4%(V/V)乙酸,按照GB 5009.156—2016的方法浸泡餐具,再参照食品安全国家标准GB 31604.15—2016和GB 31604.48—2016开展酸性条件下的迁移试验研究。结果 竹纤维密胺餐具在接触4%(V/V)乙酸时,三聚氰胺和甲醛的迁移水平远高于10%(V/V)乙醇。对单个样品而言,三聚氰胺和甲醛的迁移趋势呈正相关的规律,且长期重复接触酸性较强的食品时迁移量超标的可能性更高。随着使用次数的增加,两者的整体迁移水平逐渐升高,该规律在竹纤维添加量较高的制品中更为明显。结论 竹纤维密胺餐具中的三聚氰胺和甲醛的迁移规律在多次重复使用后仍基本一致;其中三聚氰胺的迁移水平更能反映树脂的分解情况。该类产品长期重复接触酸性食品时三聚氰胺或甲醛迁移量超标的可能性更高,尤其对于婴幼儿产品。应加强标签标识及消费者指导,杜绝使用不合规原料,促进行业良...     

竹木筷中过氧化氢在食品模拟物中迁移量的测定及其迁移规律的研究

目的:建立过氧化氢在不同食品模拟物中的测定方法,研究竹木筷中过氧化氢在不同食品模拟物中的迁移量及其迁移规律。方法:应用分光光度法测定过氧化氢,以不同食品模拟物（水基非酸性食品模拟物、水基酸性食品模拟物、酒精类食品模拟物、油基食品模拟物）中过氧化氢的质量对吸光度建立标准曲线,以相关系数、准确度和精密度为考察指标进行方法学验证;以食品模拟物的种类、迁移时间、迁移次数和迁移温度为考察因素,初步探索竹木筷中过氧化氢在食物模拟物中的迁移规律。结果:不同食品模拟物中过氧化氢建立的标准曲线相关系数均大于0.999,加标回收率范围84%~113%,加标平行样品间相对偏差（RSD）均小于10%。相同条件下,竹木筷中过氧化氢在油基模拟物中的迁移量最小;竹木筷中过氧化氢迁移存在一段快速迁移释放过程,而后转换为长时间缓慢迁移释放;过氧化氢的迁移为长时间反复迁移过程,试验至第8次仍有过氧化氢的迁移;随着温度的升高,过氧化氢迁移量会显著增加。结论:分光光度法测定竹木筷中过氧化氢在食品模拟物中迁移量准确可靠;市场部分竹木筷在不同食品模拟物中存在不同程度的过氧化氢迁移检出;其迁移规律为长时间,反复迁移的过程,增加温度可显著提高迁移速度;100 ℃煮沸处理可有效降低竹木筷中的过氧化氢的再迁移量。     

聚碳酸酯奶瓶中双酚A单体向食品模拟物迁移规律的研究

研究用食品模拟物浸泡聚碳酸酯奶瓶中双酚A的迁移规律,高效液相色谱法检测模拟物中双酚A,外标法定量。从添加回收率、精密度及线性关系等方面进行相应的方法学研究,模拟物添加量0.1～10μg/mL时,回收率为77.0%～98.7%、变异系数为5%～9.8%,在双酚A的质量浓度为0.1～10μg/mL时相关系数r=0.99996。根据该方法和欧盟有关模拟物规定的指令,检测了聚碳酸酯奶瓶中双酚A在不同模拟物和不同时间内的迁移率。     

食品接触材料中多环芳烃在食品模拟物中的迁移规律研究

采用气相色谱-质谱联用法,对食品接触材料中多环芳烃在水、乙酸(体积分数为3%)、乙醇(体积分数为10%)和异辛烷等4种食品模拟物中的迁移规律进行了研究,研究迁移量与实验的温度、时间和模拟物属性等参数的关系。结果表明:模拟物的属性对迁移行为有显著影响,迁移量随温度的升高和时间的增加而变大。     

食品接触塑料中化学成分迁移研究方法进展

塑料以其优良的物理化学性能和低廉的价格广泛应用于食品接触制品中。然而食品长期与塑料包装接触可能导致塑料中化学成分向食品中迁移,进而造成食品污染,并最终危害消费者的身体健康。故食品接触塑料中化学成分的迁移行为受到国内外政府机构和科研工作者的广泛关注。本文简述了食品接触塑料迁移实验中食品模拟物的选择、迁移实验条件的设定,以及受限物质的检测方法。并对食品接触塑料中的光引发剂、重金属元素、增塑剂等三类化学成分的迁移规律的研究进行综述。     

液相色谱串联质谱法测定纸制食品接触材料中芳香族伯胺迁移量

目的 建立纸制食品接触材料中24种芳香族伯胺迁移量的液相色谱串联质谱检测方法。方法 以不同种类食品模拟物进行模拟迁移实验, 模拟迁移液过0.22 μm滤膜测定。液相色谱使用ZORBAX-C18反相色谱柱, 以乙腈和0.1%甲酸为流动相, 在梯度条件下分析。在正离子模式下多反应监测(MRM) 采集质谱信号, 进行定性和定量分析。结果 24种初级芳香胺在50%乙醇溶液(v/v)模拟物中标准曲线的线性相关系数为0.9876~0.9999, 加标回收率为72.98%~97.88%, 相对标准偏差均在0.30%~9.90%, 定量限均小于或等于3.0 μg/kg。结论 该方法快速简便、灵敏度高、准确性好, 满足了相关法规的限量测定要求。     

网购密胺餐具的质量分析

目的 测定和分析网购密胺餐具的材质、高锰酸钾消耗量和脱色,研究迁移温度对甲醛迁移量的影响,评估网购密胺餐具的质量。方法 采集网上在售的18批次密胺餐具,通过衰变全反射（Attenuated Total Reflection） 红外法分析密胺餐具和脲醛餐具的特征吸收峰,快速区别密胺餐具和脲醛餐具。依据GB 4806.7-2016《食品安全国家标准 食品接触用塑料材料及制品》对密胺餐具高锰酸钾消耗量、脱色进行了测定和分析。依据GB 4806.6-2016 《食品安全国家标准 食品接触用塑料树脂》对密胺餐具的甲醛迁移量进行测定和分析。结果 脲醛餐具占样品总数44.4%,覆盖密胺涂层的脲醛餐具占样品总数33.3%;11.1%的样品高锰酸钾消耗量不合格;11.1%的样品4%乙酸浸泡液脱色不合格;11.1%的样品甲醛迁移量不合格（4%乙酸,70℃,2h）。结论 本次网上购买的密胺餐具高锰酸钾消耗量、脱色存在不符合GB 4806.7-2016的现象;甲醛迁移量不符合GB 4806.6-2016标准的现象,存在用脲醛餐具替代密胺餐具或是在脲醛餐具上覆盖密胺涂层以次充好的现象。     

市售密胺餐具的安全性研究

目的 测定和分析市售密胺餐具的感官、甲醛迁移量和三聚氰胺迁移量, 评估市售密胺餐具的安全性。方法 采集了市场在售的30批次密胺餐具, 依据GB 4806.6-2016《食品安全国家标准 食品接触用塑料树脂》对其感官、甲醛和三聚氰胺的迁移量进行了测定和分析。对样品进行均匀性检验, 采用单因素方差分析对结果进行统计分析。结果 23.3%的样品感官出现异常; 33.3%的样品甲醛迁移量超标; 46.7%的样品出现三聚氰胺迁移; 随着浸泡液温度的升高, 无论是甲醛还是三聚氰胺, 其迁移量都有不同程度的增加; 售价较低的样品出现问题率更高。结论 目前市场上密胺餐具的质量令人担忧, 不同价格与不同来源的餐具质量存在较大差异。消费者应选择外表光滑、平整的餐具, 同时尽量不要在高温或酸性条件下使用密胺餐具。     

Migration of formaldehyde and melamine monomers from kitchen- and tableware made of melamine plastic

Migration of one or both formaldehyde and/or melamine monomers was found in seven of ten tested melamine samples bought on the Danish market. The samples were a bowl, a jug, a mug, a ladle, and different cups and plates. No violation of the European Union-specific migration limits for melamine (30 mg kg^-1) and formaldehyde (15 mg kg^-1) was found after three successive exposures to the food stimulant 3% acetic acid after 2 h at 70°C. To investigate the effects of long-term use, migration tests were performed with two types of cups from a day nursery. Furthermore, medium-term use was studied by ten successive exposures of a plate to 3% acetic acid for 30 min at 95°C. The results indicate that continuous migration of formaldehyde and melamine takes place during the lifetime of these articles. The molar ratio of released formaldehyde to melamine was seen to decrease from 12 to about 5. This indicates that, first, the migration of residual monomers is most important, but in the long-term, breakdown of the polymer dominates. Two CEN methods were used to determine the concentration of monomers: a spectrophotometric method for formaldehyde and a UV-HPLC method for melamine.     

Migration of formaldehyde and melamine from melaware and other amino resin tableware in real life service

ABSTRACT

The migration of formaldehyde and melamine monomers has been measured on 90 samples of plastic tableware in three different situations – new articles, already used articles and artificially aged articles – by using simulant, contact times and temperatures prescribed by Commission Regulation (EU) No. 10/2011. Formaldehyde was determined by ultraviolet spectroscopy analysis of the coloured complex obtained by reaction with chromotropic acid. Melamine was measured by an ultra high performance liquid chromatography method. Fourier Transformed – Infrared Analysis was applied to characterise the plastic. The results highlighted the presence of different amino resins based on formaldehyde-melamine, urea-formaldehyde or melamine-urea-formaldehyde with different migration behaviour. The migration of monomers was related to progressive degradation of the resins. Ageing studies demonstrated that the potential degradation of the resins and the consequent migration of the monomers may continue throughout the service life of the product. The specific migration limit (SML) of melamine was exceeded after ageing.     

Effects of microwave heating on the migration of substances from melamine formaldehyde tableware

Melamine formaldehyde (MF) tableware, after undergoing repeated heating in a microwave oven for 1, 2, 3 or 5 min, was tested for migration into 3% (w/v) acetic acid, a food simulant. Overall migration (OM) consistently increased with an increasing number of heating/washing cycles, while formaldehyde was found at low concentrations or was not detectable. Unexpectedly, the 1-min series caused the most rapid increase in OM; the European Union regulatory limit of 10 mg dm^–2 was exceeded after 25 cycles. The number of cycles required to reach the OM limit rose to 29 and 67 for the 2- and 3-min series, respectively. Only 37 cycles were needed in the case of the 5-min series; however, the cumulative exposure time to microwave irradiation was relatively close to that of the 3-min series. These findings indicate that microwave heating affects the migration of MF in a significantly different manner as compared with conventional heating reported in previous studies. Fourier transform infrared spectroscopy (FTIR) spectra of MF after completing the microwave heating series show that the plastic was not fully cured, as evidenced by the absence of methylene linkages. The majority of migrants obtained from OM tests consisted of low molecular weight methylol melamine derivatives. The results indicate that microwave heating allowed demethylolation, addition and condensation reactions to occur, which was not the case when using conventional heating. This study demonstrates that microwave heating for 1–2 min in a repeated manner is of high concern in terms of consumer health. It was found that the service terms of melamine ware under microwave heating were drastically reduced, by more than 10-fold, as compared with the service terms under conventional heating. Hence, it is strongly recommended that manufacturers of MF articles provide instructions for use, e.g. “Do not use in microwave”, which should be clearly visible to consumers and not easily detachable.     

学校食堂在用密胺和不锈钢餐具检测及风险分析

目的 通过对学校食堂在用密胺和不锈钢餐具进行检测分析,并参照相关国际标准与国家标准对检测结果进行分析,以评估学校食堂在用密胺和不锈钢餐具的风险状况,为建立风险防范措施及优化现行标准提供理论依据。方法 本次检测通过对密胺餐具中甲醛迁移量、三聚氰胺迁移量;对不锈钢餐具中铅迁移量、砷迁移量、镉迁移量和镍迁移量六项指标,对食堂抽取的100批次密胺在用餐具和100批次不锈钢在用餐具样品进行风险分析。结果 本次研究共发现在用问题餐具共72批次,占比36.0%。其中在用问题密胺餐具55批次,占密胺餐具总量的55.0%;问题不锈钢餐具17批次,占不锈钢餐具总量的17.0%。密胺餐具不合格项目主要为甲醛和三聚氰胺(4%乙酸,水)的迁移量超标,不锈钢餐具不合格项目主要为铅、镉元素的迁移量超标。结论 食堂应制定密胺餐具相应的使用管理规范,设定密胺餐具的使用年限为1年以内,同时规范餐具的消毒、清洗等操作,从而有效地降低甲醛和三聚氰胺的迁移风险;应加强不锈钢餐具原料供应链管理,从源头降低风险。     

Analysis of melamine migration from melamine food contact articles

Migration of melamine has been determined for 41 types of retail melamine-ware products in Malaysia. This study was initiated by the Ministry of Health, Malaysia, in the midst of public anxiety on the possibility of melamine leaching into foods that come into contact with the melamine-ware. Thus, the objective of this study was to investigate the level of melamine migration in melamine utensils available on the market. Samples of melamine tableware, including cups and plates, forks and spoons, tumblers, bowls, etc., were collected from various retail outlets. Following the test guidelines for melamine migration set by the European Committee for Standardisation (CEN 2004) with some modifications, the samples were exposed to two types of food simulants (3% acetic acid and distilled water) at three test conditions (25°C (room temperature), 70 and 100°C) for 30 min. Melamine analysis was carried out using LC–MS/MS with a HILIC column and mobile phase consisting of ammonium acetate/formic acid (0.05%) in water and ammonium acetate/formic acid (0.05%) in acetonitrile (95?:?5, v/v). The limit of quantification (LOQ) was 5?ng/ml. Melamine migration was detected from all samples. For the articles tested with distilled water, melamine migration were [median (interquartile range)] 22.2 (32.6), 49.3 (50.9), 84.9 (89.9) ng/ml at room temperature (25°C), 70 and 100°C, respectively. In 3% acetic acid, melamine migration was 31.5 (35.7), 81.5 (76.2), 122.0 (126.7) ng/ml at room temperature (25°C), 70 and 100°C, respectively. This study suggests that excessive heat and acidity may directly affect melamine migration from melamine-ware products. However the results showed that melamine migration in the tested items were well below the specific migration limit (SML) of 30?mg/kg (30,000?ng/ml) set out in European Commission Directive 2002/72/EC.