HPLC-MS/MS法测定乳制品食品模拟物中双酚A的迁移量

建立了高效液相色谱串联三重四级杆质谱测定乳制品食品模拟物中双酚A的检测方法。以Agilent C18色谱柱进行分离,甲醇-水为流动相梯度洗脱,采用电喷雾离子源(ESI),多反映监测(MRM)负离子模式进行扫描。在选定的试验条件下,目标物的峰面积和质量浓度在1μg/L~60μg/L范围内呈良好的线性关系,最低检出限为0.20μg/L。     

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。     

食品接触材料中双酚A迁移与检测的研究进展

双酚A是一种内分泌干扰物,常被广泛应用于食品接触材料的制造中。长期暴露于双酚A环境中会导致人体免疫、生殖等系统的异常。综述了双酚A毒性、双酚A国内外检测标准与法规、食品接触材料中双酚A迁移规律与影响因素及其检测方法。     

食品包装材料中双酚A和壬基苯酚迁移量检测方法的研究

采用高效液相色谱-荧光检测法,研究不用食品模拟物(水性、酸性、酒性、脂肪性)中双酚A和壬基苯酚迁移情况。建立了不同食品模拟物中目标物的前处理方法,各类型食品模拟物对应的标准溶液线性良好,相关系数达0.999以上,双酚A和壬基苯酚迁移测定检测的方法检出限分别为0.01 mg/kg、0.01 mg/kg(水性、酸性、脂肪性食品模拟物);0.05 mg/kg、0.05mg/kg(酒性食品模拟物)。采取升温加速试验,对样品中双酚A和壬基苯酚迁移量进行了检测,结果表明,双酚A和壬基苯酚更容易在50%乙醇和异辛烷(油脂替代物)为模拟物的情况下迁出。     

食品罐内涂料中双酚A环氧衍生物的迁移及其检测

食品罐内涂料中残留的双酚-A环氧衍生物是一种环境激素,通过罐头食品进入体内,造成内分泌失衡及遗传基因变异,欧盟食品科学委员会已严令限制其使用。本文介绍了该类物质在罐头食品中的产生、迁移及检测方法。     

食品包装材料中双酚A迁移量的测定

建立采用高效液相色谱法对塑料食品包装材料中双酚A向食品模拟物迁移量的检测方法。使用4种食品模拟物：水、质量分数为4%乙酸溶液、体积分数30%的乙醇溶液和脂肪类模拟物(正己烷、异辛烷和橄榄油)。结果表明,双酚A在与食品塑料包装接触过程中,无论在何种情况下都会向食品模拟物中迁移,尤其向醇类模拟物中迁移最严重;在温度超过60℃时,双酚A向食品模拟物中的迁移率骤增;在微波加热条件,高火700W功率时双酚A向食品模拟物中的迁移速率最快。该方法检测限为0.3ng/mL,线性范围为0.5～100ng/mL,线性相关系数为0.9997,回收率在92.0%～102.4%之间,相对标准偏差≤2.84%(n=5)。     

酶联免疫法检测食品中的双酚A残留

建立检测双酚A(BPA)的间接竞争酶联免疫检测法(icELISA),探讨其在实际样品检测中的灵敏性及准确性。以抗BPA的腹水单抗建立BPA的icELISA法,利用该法对市面上聚碳酸酯(PC)制包装材料中BPA向食物的迁移量进行检测,并与高效液相色谱法检测结果相比较。BPA的icELISA法检测范围为2.817 ng/mL～1.212×106ng/mL,IC50为1 847.9 ng/mL,检测限为0.324 ng/mL,该法测定罐装鱼肉和蔬菜中BPA分别为1 015.25 ng/mL和207.22 ng/mL。     

食品塑料包装材料中光稳定剂在食品模拟物中迁移规律的研究

建立了高效液相色谱法测定食品塑料包装材料中光稳定剂UV-9和UV-531特定迁移量的分析方法.该方法采用外标法定量,两种目标化合物在相应的范围内均具有良好的线性关系,相关系数均大于0.999,检出限均为0.5μg/L.分别选取体积分数为10％、20％和50％的乙醇溶液,以及质量分数为40 g/L的乙酸溶液和正己烷5种食...     

免疫偶联物设计、合成及间接ELISA方法快速检测纯净水中双酚A的研究

设计并合成了双酚A（BPA）的免疫抗原和包被抗原,制备抗BPA多克隆抗体,并建立了间接ELISA方法用于检测瓶装纯净水中BPA的残留。首先,合成了免疫抗原DPA-BSA,并免疫新西兰大白兔得到抗BPA多克隆抗体。其次,合成结构与DPA-OVA有较大差别的包被抗原HPPA-OVA作为\     

食品包装材料中双酚A检测方法的研究进展

双酚A是一种内分泌干扰物,会导致人和动物生殖系统、免疫系统异常。由于其安全性引起世界各国研究者的广泛关注。本文就食品包装材料中双酚A的检测方法,主要包括分光光度法和荧光法、气相色谱法、气-质联用法、液相色谱法、液-质联用法、电化学分析法等,进行综述。     

食品包装用三聚氰胺成型品中甲醛迁移规律的研究

目的研究食品包装三聚氰胺成型品中甲醛迁移规律。方法采用盐酸苯肼分光光度法测定60、75和90℃三个模拟温度下甲醛从食品包装用三聚氰胺成型品中迁移至3%乙酸、15%乙醇两种模拟溶剂中的量。根据所得的实验数据,讨论了不同温度和不同食品模拟物的选择对甲醛迁移行为的影响,以及样本重复10次进行迁移实验时甲醛迁移量的变化规律。结果3%醋酸作为模拟溶剂的甲醛迁移量较15%乙醇作为模拟溶剂的高,且其迁移量随着模拟温度的升高而增多;3个温度下,2种模拟溶剂中单次迁移实验的甲醛迁移量均未超过我国国家标准的限量值和欧盟规定对其规定的特定迁移量(SML)2.5 mg.dm-2,而以3%醋酸作为模拟溶剂的甲醛的10次迁移实验的总量均超过欧盟对甲醛的特定迁移量。结论食品包装用三聚氰胺成型品不宜在酸性和高温条件下使用。     

Tailoring fatty food simulants made from solvent mixtures (2): determining the equivalent migration behaviour of olive oil and of solvents in the case of polyolefins

It is suggested that solvent mixtures consisting of an ester and of an inert solvent can be used as fatty food simulants capable of having the same migration behaviour as olive oil with plastics. Migration tests carried out with low-density polyethylene for 20 and 48h in an 8 and 5% mixture of tert-butyl acetate in ethanol respectively gave results equivalent to those obtained with olive oil after 10 days at 40°C. The use of solvent mixtures facilitated the analysis and improved detection limits, giving good repeatability. Furthermore, the more rapid migration in solvent mixtures can be particularly useful for industrial controls as alternative test methods.     

食品包装中纳米材料向食品或食品模拟物迁移的研究现状

纳米复合材料在食品包装材料中已开始大规模应用,然而纳米复合包装材料中的纳米成分有向食品迁移的动力和趋势,现已成为食品安全隐患的重要组成部分。结合国内外的研究,对食品包装材料中纳米成分迁移的试验研究、数学模型和表征方法的研究现状和趋势加以综述,为科研工作者的理论和试验研究提供参考。     

食品模拟体系中淀粉基膜材增塑剂的迁移

本文采用酯化淀粉以三乙酸甘油酯为增塑剂,经流延法制备了酯化淀粉薄膜,并利用傅里叶红外光谱衰减全反射技术(ATR-FTIR)和热重分析仪(TGA)分析了淀粉基膜材与不同食品模拟体系接触后其表层增塑剂和整体增塑剂的变化情况。结果表明,基于与淀粉基膜材、增塑剂之间的亲和性差异,食品模拟体系对淀粉基膜材产生不同的溶胀作用,导致不同程度的增塑剂迁移;与淀粉基膜材亲和性越高的食品模拟体系,对淀粉基膜材表层和内部的溶胀更迅速,并可溶解更多的增塑剂分子,从而导致淀粉基膜材中更大程度的增塑剂迁移;表层增塑剂和整体增塑剂的迁移情况差异表明,溶剂溶胀和增塑剂迁移由膜材表层向内部发生。基于以上结果可推断,在实际应用过程中,选择合适的应用领域、设计调整材料结构可主动抑制增塑剂迁移,实现这类新型包装材料的安全使用。     

Characterizing the migration of antioxidants from polypropylene into fatty food simulants

The migration (diffusion and equilibrium) processes of antioxidants (AOs) from polypropylene (PP) films of different thicknesses into n-heptane and 95% ethanol as fatty food simulants were analysed at 20, 37 and 60°C. Heptane fully extracted the AOs from the polymer while a partition equilibrium described the migration to ethanol. The kinetics of migration were also studied via the diffusion coefficients. As expected, diffusion was found to be faster when the polymer was in contact with heptane, due to polymer swelling by the solvent. The kinetics of the process in ethanol was described by different theoretical expressions which are discussed. Equations disregarding partition equilibrium failed to describe the process and the diffusion coefficient values obtained through them were much smaller than the actual ones and dependent on film thickness. The results also showed the significance of food simulant selection in the analysis of food-packaging interactions and migration variability with thickness.     

Determination of bisphenol A in, and its migration from, PVC stretch film used for food packaging

Bisphenol A (BPA) is used as an additive in polyvinyl chloride (PVC) products, including stretch films used for food packaging. The BPA contents were investigated of several brands of stretch film bought locally but marketed internationally or throughout Spain and which were presumably produced at different manufacturing plants. Their major components were identified by FTIR (Fourier Transform Infrared Spectrometry) and horizontal attenuated total reflectance, and the migration of BPA from these materials into the standard European Union food simulants was determined by high-performance liquid chromatography (HPLC) using both fluorescence (FL) and ultraviolet (UV) detection, the identity of the analyte being confirmed by gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-mass spectrometry (LC-MS). The two HPLC detection methods had different detection limits (30 μg l^-1 for UV, 3 μg l^-1 for FL), but afforded virtually identical BPA determinations for the samples tested. BPA contents ranging from 40 to 100 mg kg^-1 were found in three of the five PVC-based films analysed, and a content of 500 mg kg^-1 was found in a fourth; for these determinations, extraction into acetonitrile was used. In standard tests of migration into water, 3% acetic acid and olive oil over 10 days at 40°C, migration from a given film was in all cases greatest into olive oil. Migration from the films with non-zero BPA contents ranged from 3 to 31 μg dm^-2, values higher than those reported for many other food-contact materials, but lower than the European Union specific migration limit for BPA. PVC stretch film nevertheless may make a significant contribution to contamination of foodstuffs by BPA, and should be taken into account in estimating BPA intake or exposure to this substance.     

食品模拟体系中淀粉基膜材增塑剂迁移的动力学模型

本文以高取代度酯化淀粉为基材、以三乙酸甘油酯为增塑剂制备了淀粉基膜材。以热重分析技术(TGA)分析了膜材与食品模拟体系接触后增塑剂的变化情况,在此基础上对用增塑剂向食品体系的迁移过程进行了整体动力学分析和扩散模型分析。结果表明,在与淀粉基膜材亲和性较低的4%乙酸体系中,增塑剂的整个迁移过程更符合整体一级动力学,增塑剂短期迁移过程遵循菲克第二扩散定律,而后续的迁移遵循非菲克扩散定律;在与淀粉基膜材具有更高亲和性的65%乙醇和正己烷体系中,增塑剂迁移遵循非菲克扩散定律,且长期迁移更显著。以上结果说明,基于食品模拟体系与膜材的亲和性差异,增塑剂通过溶胀层向食品模拟体系的迁移呈现不同的动力学特点,且因膜材/模拟体系相互作用的影响而改变。     

聚氯乙烯类食品包装材料中三甲基锡向食品模拟物的迁移规律

目的：建立聚氯乙烯类包装材料和食品模拟物中三甲基锡的超高效液相色谱-串联质谱（ultra performanceliquid chromatography-tandem mass spectrometry,UPLC-MS/MS）联用测定方法。用该方法研究聚氯乙烯中的三甲基锡向食品模拟物的迁移规律。方法：聚氯乙烯包装材料样品用乙酸乙酯提取。食品模拟物经阳离子固相萃取柱净化富集,洗脱液水浴条件下氮气吹干,残渣用流动相溶解,旋涡混匀,过0.22 μm微孔滤膜,经C18色谱柱完成分离,MS/MS仪上采用多反应监测正离子模式测定三甲基锡,外标法定量。在设定的不同温度条件下,将聚氯乙烯包装材料浸泡于食品模拟物中,于不同的时间点移取浸泡液,经前处理后测定三甲基锡迁移量。结果：三甲基锡在0.1～100.0 μg/L范围内线性关系良好（相关系数r=0.999 8）,检出限为0.02 μg/L。在1.0、10.0、50.0 μg/L 3 个添加水平范围内的平均回收率为90.6%～97.3%,相对标准偏差不高于6.9%。测定结果显示,三甲基锡迁移量在水模拟物中为0.19～1.65 μg/L、在体积分数10%乙醇模拟物中为0.19～9.89 μg/L、在3 g/100 mL乙酸模拟物中为0.11～9.96 μg/L、在正己烷模拟物中为0.15～3.54 μg/L。结论：建立的阳离子固相萃取-UPLC-MS/MS联用法测定食品模拟物中三甲基锡的方法快速简单、准确有效,三甲基锡在体积分数10%乙醇溶液和3 g/100 mL乙酸溶液迁移量较高,且随温度升高、时间延长,迁移量增加,一定时间后达到迁移平衡。     

Influence of solvent absorption on the migration of Irganox 1076 from LDPE

The effect of solvent absorption on additive migration was studied by relating the diffusion coefficient ( D ) of Irganox 1076 to the maximum solvent absorption of different solvents in low-density polyethylene (LDPE) film. Solvents tested were ethanol, isopropanol, isooctane, ethylacetate, cyclohexane, tributyrin, tricaprylin and olive oil. Diffusion and partition coefficients were determined by fitting the migration curves, i.e. the concentration of Irganox 1076 in solvent as a function of time, with Fick's diffusion equation. The results for the low molecular weight solvents show that with increasing maximum solvent absorption, D of Irganox 1076 is increasing as well. This trend is not observed for the two triglycerides and olive oil. In spite of absorption, no increase in D was observed. The obtained result is the basis of an extended predictive migration model that, besides migrant and polymer properties, is also based on the maximum solvent absorption in the polymer.