塑料食品包装中罗丹明B迁移量的分析

针对塑料食品包装中罗丹明B迁移量的分析,本文首先建立了水、4%(体积分数)乙酸、20%(体积分数)乙醇和50%(体积分数)乙醇水溶液以及橄榄油五种食品模拟物中罗丹明B的高效液相色谱-荧光检测器分析方法。四种水性食品模拟物中,罗丹明B含量在0.001～0.200 mg/L范围内线性良好,在橄榄油中,罗丹明B含量在0.005～0.200 mg/kg范围内线性良好。标准添加试验结果表明方法回收率较高,相对标准偏差较低,准确度和稳定性较好。验证后的方法运用于实际样品分析,在50个市售塑料食品包装中,3个包装在实际使用条件下的迁移试验数据表明,罗丹明B迁移量在0.002～0.023 mg/kg之间。     

顶空气相色谱法测定与食品接触的ABS材料中苯乙烯迁移量

探讨了与食品接触的丙烯腈-丁二烯-苯乙烯共聚物(ABS)材料在蒸馏水、3%乙酸、10%乙醇、20%乙醇、50%乙醇5种水性模拟物中苯乙烯迁移量的测定方法。结果表明:5种不同模拟物中苯乙烯在0.02~0.32mg/L浓度范围内线性关系均良好(相关系数r≥0.995),检出限(信噪比S/N=3)均为0.01 mg/L。目标物在0.04~0.16 mg/L 3个添加水平下,平均回收率为81.5%~102%,相对标准偏差(n=6)为3.15%~8.32%。该方法操作简单、快速、准确,能够满足食品接触材料的日常检验要求。     

食品接触材料中2,2,4,4-四甲基-1,3-环丁二醇迁移量的测定

采用气质联用技术,建立了食品接触材料中2,2,4,4-四甲基-1,3-环丁二醇迁移量的分析方法。样品经4%乙酸、10%乙醇、20%乙醇、50%乙醇、橄榄油、95%乙醇、异辛烷浸泡后得到浸泡溶液,经有机溶剂提取后供气质联用仪分析,外标法定量。水基、酸性、乙醇类、橄榄油食品模拟物及化学替代溶剂中2,2,4,4-四甲基-1,3-环丁二醇的检出限在0.008～0.080 mg/L之间,方法的平均回收率在90.2%～107.8%之间,相对标准偏差在2.61%～9.04%之间。该方法前处理简单,检测速度快,灵敏度高,满足食品接触材料中2,2,4,4-四甲基-1,3-环丁二醇迁移量的分析要求。     

固相微萃取气质联法测定丙烯腈迁移量

丙烯腈单体是剧毒化学品,为了快速,高效,绿色的检测食品接触材料中的丙烯腈迁移量,对SPME-GCMS的条件如萃取时间温度,萃取纤维类型,解析时间和GCMS条件进行优化,建立了自动固相微萃取-气象色谱-质联用谱(SPMEGCMS)测定食品模拟夜中的丙烯腈迁移量的分析方法,方法线性范围0.01~0.20 mg/kg,线性相关系数大于0.999,检出限达到0.01 mg/kg,重复性实验得到相对标准偏差小于5%,加标回收率为85%~115%.满足食品接触材料中的丙烯腈迁移量检测要求。     

食品接触材料成型品中的苯乙烯单体迁移风险分析

通过研究食品接触材料(聚苯乙烯(PS)、丙烯腈-苯乙烯共聚物(AS)及丙烯腈-丁二烯-苯乙烯共聚物(ABS))成型品样本的4种食品模拟物(水、3%乙酸、10%乙醇、葵花籽油)中苯乙烯单体的迁移情况,并进行风险分析,初步确定食品接触材料成型品中苯乙烯单体迁移的风险等级。通过顶空-气相色谱质谱联用法测定食品模拟物中苯乙烯单体的迁移量,并计算苯乙烯单体的日累计暴露量,结合专家评估的方式进行风险分析。结果表明:苯乙烯单体在水、3%乙酸、10%乙醇、葵花籽油4种食品模拟物中均有迁移,在葵花籽油食品模拟物中苯乙烯单体迁移量较高,其次是水、10%乙醇、3%乙酸;所采集样本中苯乙烯单体日累计暴露量小于0.01 mg/(d·kg),且低于JECFA规定的苯乙烯安全摄入量。结合专家评估结果,最终确定食品接触材料成型品中的苯乙烯单体迁移风险等级为L级(低风险)。     

聚苯乙烯杯中苯乙烯在豆制品、粥类食品和醇类模拟物中的迁移对比

选取苯乙烯迁移量作为测试指标,对比了聚苯乙烯杯中残留苯乙烯在真实食品及醇类食品模拟物中的迁移量,分析确认适合这几类中国特色食品的模拟物。采用顶空?气相色谱法测定苯乙烯在3类真实食品、10 %乙醇（体积分数,下同）和20 %乙醇中的迁移量,采用高效液相色谱法测定苯乙烯在50 %乙醇和95 %乙醇中的迁移量。结果表明,豆类饮料中苯乙烯迁移量介于其在20 %乙醇和50 %乙醇中的迁移量之间;豆腐和粥中苯乙烯的迁移量接近10 %乙醇和20 %乙醇,均远低于50 %乙醇;根据食品接触材料及制品的食品模拟物适用性原则,应选择与食品迁移量接近或大于食品迁移量的模拟物,建议豆类饮料选择50 %乙醇作为模拟物,豆腐类食品和粥类食品选择20 %乙醇作为模拟物,相关结果可为食品安全国家标准的修订提供参考。     

超高效液相色谱法测定食品包装材料中五种抗氧化剂迁移量

采用水基模拟物(蒸馏水、3%乙酸水溶液、10%乙醇水溶液)和油脂模拟物(异辛烷),建立了超高效液相色谱法测定食品包装材料中BHA、BHT、DLTP、DMTP、抗氧化剂CA等5种抗氧化剂迁移量的检测方法。结果表明:在2.00~100.00 mg/kg浓度范围内,具有良好的线性关系,相关系数≥0.999 5;检出限0.50~1.00 mg/kg、定量限范围1.50~3.00 mg/kg;加标回收率在80.7%~115.7%之间,相对标准偏差(RSD)在0.5%~2.8%之间,表明该方法简便、准确,可用于食品包装材料中5种抗氧化剂迁移量的同时检测。     

固相微萃取-气相色谱/质谱法测定塑料食品接触材料中5种丙烯酸酯类单体迁移量

建立了固相微萃取-气相色谱/质谱联用法(SPME-GC/MS)测定塑料食品接触材料的水性模拟液中5种丙烯酸酯类单体的分析方法。并且对萃取纤维、解吸时间、萃取时间、萃取温度、振荡速率、离子强度和顶空体积等固相微萃取条件进行了优化。结果表明:5种丙烯酸酯类单体能达到良好的分离,定量限(信噪比=10)为0.01~0.005μg/L,相关系数(R)大于0.999,平均回收率及相对标准偏差(n=5)分别在89.47%~99.49%和0.62%~5.51%的范围内。所建方法操作简便、灵敏度高、准确度好,能够满足塑料食品接触材料中5种丙烯酸酯类单体迁移量的检测需要。     

气相色谱-串联质谱法测定聚萘二甲酸乙二醇酯中2,6-萘二甲酸二甲酯的迁移量

建立了气相色谱-串联质谱法测定食品接触材料聚萘二甲酸乙二醇酯中2,6-萘二甲酸二甲酯迁移量的方法。采用二氯甲烷对水、质量浓度为30 g/L的乙酸、体积分数10%、20%、50%的乙醇五种食品模拟物中的2,6-萘二甲酸二甲酯进行液液萃取后进样分析。结果表明:2,6-萘二甲酸二甲酯标准溶液的检出限为0.005 mg/L,在0.02～0.50 mg/L范围内线性良好。对5种不同食品模拟物中2,6-萘二甲酸二甲酯进行加标回收实验,平均回收率为96.1%～105.0%,相对标准偏差(n=6)为0.9%～3.7%。实际样品分析结果表明,在50%乙醇食品模拟物中,2,6-萘二甲酸二甲酯的迁移量最高。该方法灵敏度高、抗干扰能力强、定量准确、重现性好,能够满足聚萘二甲酸乙二醇酯中2,6-萘二甲酸二甲酯迁移量测定要求。     

气相色谱-串联质谱法测定食品接触材料中邻苯二甲酸酯含量和迁移量

文章建立气相色谱-串联质谱法,测定食品接触材料中邻苯二甲酸二异辛酯（DIOP）和邻苯二甲酸二异癸酯（DIDP）的含量和迁移量。采用水、4%乙酸、10%乙醇、20%乙醇、50%乙醇、95%乙醇和油脂替代物正庚烷进行迁移试验,在迁移试验温度为60℃,迁移时间为10 d条件下,对检测方法的精密度（RSD）、准确度等进行探究。结果表明：含量测定线性相关系数r2≥0.999、加标回收率范围为93.8%～105.6%、RSD范围为1.0%～2.2%。迁移量测定线性相关系数r2≥0.999、加标回收率范围为92.4%～108.3%、RSD范围为0.2%～5.7%。此方法灵敏度高、准确度高,适用于测定食品接触材料中DIOP和DIDP的含量和迁移量。     

Effect of temperature and type of food simulant on antioxidant stability

Additive migration levels in food simulants from polimeric materials that are intended to be into contact with food can be affected by additive stability under the migration test conditions. In this work, the stability of some phenolic antioxidants and one oxidized phosphite antioxidant was studied in four food simulants: distilled water, 3% (w/v) acetic acid, 10% (v/v) ethanol, and the fatty food simulant olive oil, under different temperatures 5, 40, and 70°C, during ～20 days. Samples were analyzed by reversed‐phase high performance liquid chromatography (HPLC) with UV diode‐array detector. In general, antioxidants appeared to be more stable in olive oil than in the aqueous simulants. Among aqueous simulants, water and 10% ethanol allowed the highest stability of antioxidants at low temperatures. The 3% acetic acid allowed good stability for the lowest phenolic compounds even at high temperatures, but the highest molecular weight compounds decomposed very fast even at low temperatures. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 656–663, 2006     

化妆品包装材料中邻苯二甲酸双(2-乙基己基)酯迁移量的测定

建立了化妆品包装材料中邻苯二甲酸双(2-乙基己基)酯迁移量(DEHP)的气相色谱质谱检测方法。化妆品包装材料样品采用不同模拟物在不同条件下浸泡后,浸泡液经正己烷萃取,气相色谱质谱联用仪分析,外标法定量。在优化的条件下,DEHP在0.01~10.0 mg/L浓度范围内线性关系良好,相关系数为0.999 3,方法检出限为0.10 mg/L。在空白样品中添加低、中、高3个浓度水平时,平均加标回收率在90%~110%之间,相对标准偏差在2.4%~8.2%之间。方法简单快速、灵敏可靠,可满足化妆品包装材料中DEHP迁移量的检测需求。对阳性样品中DEHP的迁移行为进行研究,结果表明DEHP迁移量随着浸泡液中乙醇比例的增大和浸泡时间的增加而增加。     

Physical–chemical and structural stability of PHBV/wheat straw fibers based biocomposites under food contact conditions

This aricle aims at investigating for the first time the ability of using poly(3-hydroxylbutyrate-co-3-hydroxyvalerate) (PHBV)/wheat straw fibers (WSF) biocomposites as food contact materials for packaging applications. For that purpose, the impact of the filler size and content on overall migration and mechanical properties was assessed under standardized testing conditions using the food simulant liquids (FSL). Very high overall migration values were noticed in the case of hydrophilic FSL, that is, water, acetic acid 3% (wt/vol), ethanol 20% (vol/vol), and ethanol 95% (vol/vol), related to the leaching of water extractable components of WSF. Low migration values were obtained in contact with isooctane and olive oil, demonstrating the possibility of using biocomposites in contact with fatty products. To answer the lack of methodologies to simulate different types of food for which PHBV-based composites could be more specifically dedicated, including food products of low or intermediate water activity such as fruits and vegetable, bread, and cheese, a new range of new solid food models based on agar-agar gels have been developed. Results showed that the water activity (a_w) was the main parameter governing the overall migration of PHBV/WSF materials, suggesting that such composite materials could only be used as food contact materials in the case of food products with an a_w equal or lower than 0.90.     

气相色谱-质谱法测定硅油纸中二异丙基萘(DIPN)迁移量

建立了快速检测硅油纸中二异丙基萘(DIPN)迁移量的气相色谱-质谱法。样品采用50%乙醇和异辛烷作为预期接触含酒精类和油性的食品模拟物,40℃进行2 h的迁移试验。迁移后的模拟液加入内标液经过超声、混匀后取上清液直接进样,选择性离子模式扫描,内标法定量。结果表明,二异丙基萘(DIPN)迁移量的线性范围0.1~100 mg/kg、检出限0.5 mg/kg、定量限(以信噪比≥10计)1.0 mg/kg;在3个加标水平下,平均加标回收率82.0%~95.34%、相对标准偏差2.08%~3.95%(n=6)。检测方法具有优异的灵敏度和稳定性,满足对硅油纸中二异丙基萘(DIPN)迁移量的分析检测和准确定量。     

Type of polypropylene material significantly influences the migration of antioxidants from polymer packaging to food simulants during microwave heating

Three different polypropylene materials, polypropylene homopolymer (PP), propylene‐ethylene random copolymer (PP‐R), and propylene‐ethylene copolymer (PP‐C) are commonly used in plastic containers designed for microwave heating of food. Migration of antioxidants, Irganox 1010 and Irgafos 168, from PP, PP‐R, and PP‐C during microwave heating in contact with different food simulants was investigated by utilizing microwave assisted extraction (MAE) and high performance liquid chromatography (HPLC). The polypropylene material significantly influenced the migration rate, which decreased in the order of increasing degree of crystallinity in the materials. PP homopolymer was the most migration resistant of the studied materials especially in contact with fatty food simulants. The use of isooctane as fatty food simulant resulted in rapid depletion of antioxidants, while migration to another fatty food simulant, 96% ethanol, was much more limited. Migration to aqueous and acidic food simulants was in most cases under the detection limits irrespective of microwaving time and temperature. The diffusion coefficients were similar to what have been found previously under similar conditions but without microwaves. The effect of swelling was shown by the large increase in the calculated diffusion coefficients when isooctane was used as food simulant instead of 96% ethanol. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

食品接触用生物降解塑料购物袋材质鉴别与总迁移量研究

采用红外光谱仪（FTIR）对市售的6种食品接触用生物降解塑料购物袋（1^#~6^#）材质进行鉴别,测试了其在不同浸泡条件下的总迁移量,并对部分样品的蒸发残渣成分进行了表征。结果表明,2^#与4^#样品材质定性结果与其标注材质不一致;生物降解塑料购物袋总迁移量远大于传统聚乙烯（PE）塑料购物袋,2^#~6^#样品在4 %（体积分数,下同）乙酸模拟液中浸泡及1^#~6^#样品在95 %乙醇模拟液中浸泡时的总迁移量均超过限量要求（10 mg/dm²）,说明生物降解塑料购物袋直接接触食品存在一定食品安全风险;样品中的PBAT能在95 %乙醇中溶解;样品中掺杂的CaCO₃在4 %乙酸模拟液中出现了大量迁移,这是由于CaCO₃本体发生迁移及CaCO₃与乙酸发生反应生成了乙酸钙;淀粉（ST）颗粒在水中会发生糊化脱落,而乙酸进入ST颗粒中会破坏ST的分子结构,导致掺杂ST的生物降解塑料购物袋总迁移量显著增大。     

Ethanol shock enhances the recovery of anthocyanin from lowbush blueberry

Deactivation of polyphenol oxidase (PPO) in natural products is essential for downstream processing of functional molecules used as food or food additives, particularly those served as antioxidants. In the present work, we identified two proteins with PPO activity from lowbush blueberry using ammonium sulphate precipitation and chromatography procedures. Deactivation of these proteins was studied using aqueous solutions of ethanol of different concentrations. The PPO activity was recovered after ethanol removal for the protein samples previously soaked in a low concentration ethanol solution. A complete and unrecoverable deactivation of the proteins was achieved using ethanol with concentration over 70% (v/v), as manifested by the significant changes in circular dichroism (CD) and fluorescence spectroscopy measurements. Based on these findings, we propose a new extraction process for blueberry anthocyanin, in which an ethanol shock, i.e. soaking blueberry fruit in a 70% (v/v) ethanol solution for 1 h, is implemented before subsequent procedures. This new process increases the anthocyanin yield by 55% in comparison to that without the ethanol shock.     

食品接触材料中三乙醇胺迁移量的测定

建立了食品接触材料中三乙醇胺迁移量的液相色谱-串联质谱法(LC-MS/MS)测定方法。食品接触材料浸泡液以氨基柱BEH Amide(50 mm×2.1 mm,1.7μm)作为分离色谱柱,以乙腈-水溶液为流动相,采用梯度洗脱的方式分离,在电喷雾离子源下以多反应监测(MRM)模式进行检测,外标法定量。在优化的条件下,三乙醇胺在5.0~100μg/L范围内线性关系良好,相关系数大于0.999,检出限(LOD,S/N=3)和定量限(LOQ,S/N=10)分别可达1.0和5.0μg/kg。在低、中、高3个水平加标浓度下的回收率为97.6%~100.8%,相对标准偏差(RSD)为0.7~1.7%,本方法简单方便、快速灵敏、准确可靠,可满足相关检测需求。     

Ethanol shock enhances the recovery of anthocyanin from lowbush blueberry

Deactivation of polyphenol oxidase (PPO) in natural products is essential for downstream processing of functional molecules used as food or food additives, particularly those served as antioxidants. In the present work, we identified two proteins with PPO activity from lowbush blueberry using ammonium sulphate precipitation and chromatography procedures. Deactivation of these proteins was studied using aqueous solutions of ethanol of different concentrations. The PPO activity was recovered after ethanol removal for the protein samples previously soaked in a low concentration ethanol solution. A complete and unrecoverable deactivation of the proteins was achieved using ethanol with concentration over 70% (v/v), as manifested by the significant changes in circular dichroism (CD) and fluorescence spectroscopy measurements. Based on these findings, we propose a new extraction process for blueberry anthocyanin, in which an ethanol shock, i.e. soaking blueberry fruit in a 70% (v/v) ethanol solution for 1 h, is implemented before subsequent procedures. This new process increases the anthocyanin yield by 55% in comparison to that without the ethanol shock.