高效液相色谱法同时测定食品塑料包装材料中8种邻苯二甲酸酯的含量

建立检测塑料包装材料中8种邻苯二甲酸酯类(PAEs)的高效液相色谱法,并采用所建立的方法分析了7种塑料材质、包装不同类型食品的27个塑料包装材料中的PAEs含量,结果发现所有抽检样品中均含有DBP,且44%的样品中含有DEHP,其中1个样品还含有BBP,其他的PAEs未被检出,说明我国目前食品塑料包装材料所用增塑剂主要以DBP和DEHP为主;DBP的含量范围为22.89～267.6mg/kg,而DEHP的含量范围为0.33～899.8mg/kg,其中PET和HDPE两种包装材料中含有很高量的DEHP。     

毛细管气相色谱法测定塑料包装及包装内食品中酞酸酯

建立了用毛细管气相色谱-氢火焰离子化检测器测定塑料食品袋及袋内包装食品中5种酞酸酯(邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二正辛酯(DOP)和邻苯二甲酸二(2-乙基己基)酯(DEHP))的方法。样品用无水乙醇超声提取,经干燥脱水过0.45μm滤膜过滤,直接注入气相色谱仪进行分析。用保留时间定性,外标法定量。5种酞酸酯的回收率为71.5%～125.5%;精密度(RSD)为1.6%～3.2%;DMP、DEP、DBP、DOP和DEHP的检测限分别为0.18、0.13、0.13、0.15和0.14ng。该方法准确度和灵敏度高,样品用量少,前处理简单,可同时测定塑料食品袋及包装内食品中5种酞酸酯。     

美国发明超洁净塑料袋

美国近日发明了一种超净塑料袋。这种塑料袋可以使内装物置于无尘环境中，而且其本身所散发出化学气体不会对内装物造成腐蚀。精密光仪器和电子总线制造商是超净塑料包装袋的主要客户，包装对象小到小零件、微型装置，大至对粉尘敏感的总线制造设备和涡轮发动机。据悉，这种包装袋得灵感来自于近年来一些行业对塑料包装袋内部洁净度的越来越高的要求，由此带来了超净塑料包装袋市场的起步和繁荣。     

PVC薄膜中邻苯二甲酸二乙基己酯对食品迁移的研究

邻苯二甲酸二乙基己酯(DEHP)作为增塑剂能改进聚合物的性能,特别是聚氯乙烯(PVC)一般添加该物质来生产薄膜。DEHP有害身体健康。当包装材料接触到食品时候,DEHP会通过迁移污染被包装物。研究了PVC塑料膜中增塑剂DEHP迁移到几种溶液。PVC塑料膜分别浸入100%正己烷、100%大豆色拉油、20%乙醇、10%食盐水、4%醋酸、蒸馏水中,在常温(25℃)下放2h、1d、2d、3d、4d、5d,溶液中DEHP浓度用高效液相检测。PVC薄膜分别浸入到100%正己烷、100%大豆在25、4、-18℃下放置1、2、3、4、5d。小包子蒸熟后马上用PVC塑料膜包装常温放置。猪肉用PVC塑料膜包装贮藏于4℃。西兰花和绿豆发芽后种植1周,通过覆盖地膜研究PVC塑料膜中DEHP迁移到植株中。研究结果显示:PVC塑料膜中DEHP最大迁移的溶液是100%正己烷,100%大豆色拉油、20%乙醇溶液中的迁移量也比较大,10%食盐水、4%醋酸、蒸馏水溶液中迁移量很少;DEHP对100%正己烷和100%大豆色拉油的迁移都是随温度上升而增加。PVC塑料膜中DEHP在30min内迁移到热的小包子已经很多。用PVC塑料膜包装猪肉在4℃下,...     

气相色谱法测定食品塑膜包装材料中增塑剂邻苯二甲酯的研究

本文对食品塑膜包装材料中增塑剂邻苯二甲酸二辛酯(DEHP)的气相色谱测定法进行了研究,提出用索氏萃取法以乙醚萃取DEHP或用甲醇沉淀法将塑料基质从试液中除去,分离出DEHP,然后以邻苯二甲酸二戊酯为内标,在交联甲基硅酮毛细管柱上,用FID检测器作气相色谱定量测定。萃取法和沉淀法的平均回收率分别为96.5%和85.3%。两方法的变异系数约为2%,最小检测量约2×10~(-3)μg。沉淀法的回收率略低于萃取法,因此在沉淀过程中,DEHP有被沉淀物包留的可能,若沉淀小心进行,避免产生凝絮状沉淀物则包留现象可获得改善。     

塑料购物袋国标将于6月1日前正式出台

正日前,国家标准委员会相关负责人表示,塑料购物袋新国标将于6月1日前正式出台,此标准由国家塑料标准化委员会负责起草,将是首部专门针对塑料购物袋的强制性国标。据悉,塑料购物袋国标的部分内容为:食品用塑料袋须在显眼位置注明"食品用"等字样,并打上QS标识;国标规定塑料袋的单面厚度不得低于0.025毫米;在尺寸方面,长度和宽度的误差不得超过2%,外观应质地均匀、无皱褶、无污迹、无气泡;塑料袋     

食品塑料包装材料中DEHP的风险评估

邻苯二甲酸二（2-乙基己基）酯（DEHP）是一种常用的增塑剂,广泛应用于塑料的生产中,用以改善塑料的柔韧性、曲挠性和拉伸性。但多项研究表明,DEHP是一类环境雌激素,具有生殖毒性、发育毒性和致癌作用,食品在与含有DEHP的包装材料或容器接触时, DEHP单体会迁移溶入到食品当中,从而污染食品,危害人类身体健康。近年来,国内外发生了多起因DEHP导致的食品安全事件,引起了消费者的恐慌,DEHP的危害也受到了全社会的广泛关注。     

白酒中两种常见塑化剂快速定量方法的研究

根据2011年6月卫生部签发的551号文件《卫生部办公厅官员通报食品及食品添加剂中邻苯二甲酸酯类物质最大残留量的函》[1]规定,建立了气相色谱-质谱同时测定白酒中相关塑化剂含量的检测方法。特别对影响白酒样品中塑化剂提取的各种因素和多种前处理方法进行比较,并进行优化处理,最终使本方法能够快速准确测定白酒中的塑化剂含量,具有准确度高、操作简便、成本低等优点。试验结果显示,在S/N=10条件下,DBP、DEHP的定量下限分别为0.04mg/L、0.03mg/L,平均加标回收率为94.4%~108.3%,精密度试验R SD均小于6%,满足常规定量分析要求。     

塑料笔杆中邻苯二甲酸酯的检测及风险分析

通过气相色谱质谱法对塑料笔杆中邻苯二甲酸二丁酯(DBP)、邻苯二甲酸丁苄酯(BBP)、邻苯二甲酸二(2-乙基)己酯(DEHP)、邻苯二甲酸二正辛酯(DNOP)、邻苯二甲酸二异壬酯(DINP)、邻苯二甲酸二异癸酯(DIDP)六种邻苯二甲酸酯进行检测,结果发现DEHP的检出率为40%,DBP的检出率为10%,BBP、DINP、DIDP的检出率为5%;并对检测结果进行风险分析,结果发现8批次DEHP中有3批次暴露量的值高于参考剂量0.02 mg/Kg/d,危害商值大于1的样品也有3批次。由此可见,塑料笔杆中邻苯二甲酸酯对儿童的身体健康造成影响的可能性比较大,为保证儿童的身体健康,建议购买质量好的塑料笔杆。     

超声波萃取-气相色谱法测定塑料袋袋装食品中邻苯二甲酸酯

采用超声波萃取-气相色谱法测定经塑料食品袋盛装后食品中邻苯二甲酸酯(PAEs)含量。取烧饼、麻花和馒头样品用同种塑料食品袋与纸袋分别盛装30 min,进行检测。PAEs添加回收率在84．1％～107．8％之间,标准偏差在1．6％～6．7％之间。测定结果表明,经塑料袋盛装后食品PAEs含量均有不同程度提高:PAEs对温度高食品污染程度大;且PAEs对油脂含量高的食品污染程度比油脂含量低的污染程度大;PAEs对食品表面污染程度大于内部。     

固相萃取- 气相色谱法测定食品包装材料中邻苯二甲酸酯类物质

建立采用固相萃取-气相色谱法同时分析检测邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二环己酯(DCHP)、邻苯二甲酸丁基苄基酯(BBP)和邻苯二甲酸二-2-乙基己酯(DEHP)4种邻苯二甲酸酯类物质的方法。研究塑料包装材料中邻苯二甲酸酯类在水、65%乙醇、4%乙酸、正己烷4种模拟液中的溶出及利用固相萃取技术对浸出液进行富集的情况,考察气相色谱操作条件对4种邻苯二甲酸酯类物质分离的影响。结果表明,该方法具有良好的线性相关性,线性相关系数在0.9986～0.9994之间;回收率在80.63%～95.50%之间;DBP、BBP、DCHP和DEHP的检测限分别是0.050、0.010、0.055μg/mL和0.012μg/mL。该方法样品预处理简便,测定方法灵敏、可靠,可用于食品包装材料中邻苯二甲酸酯类的监测。     

基质固相分散-高效液相色谱法测定蔬菜中邻苯二甲酸酯类

研究了蔬菜中的邻苯二甲酸二丁酯(di-n-butyl phthalate,DBP)和邻苯二甲酸二辛酯(di-2-ethylhexyl phthalate,DEHP)基质固相分散处理和高效液相色谱测定方法。蔬菜样品经弗罗里硅土和石墨化碳黑研磨均匀后,用乙酸乙酯淋洗净化。结果表明:DBP和DEHP在0.1～10mg/L范围内具有良好的线性,样品的添加回收率在86.2%～91.4%,相对标准偏差2.9%～4.8%。该方法操作简便经济,分析速度快,可适用于大批量样品分析。     

毒理学关注阈值方法的建立及其在食品接触材料评估中的应用

目的以邻苯二甲酸二(2-乙基己基)酯(DEHP)为模式化学物,建立可用于食品接触材料的毒理学关注阈值(TTC)风险评估方法。方法建立基于Cramer结构分类的TTC决策树方法;利用Cramer结构分类流程和Toxtree软件对DEHP进行Cramer结构分类;利用2002年中国居民营养与健康状况调查数据和部分食物中DEHP的监测数据,估计我国不同年龄组人群通过饮料、植物油、发酵乳、方便面、果冻、果酱的DEHP暴露量,并按照TTC决策树方法对DEHP进行风险评估;同时,采用传统的风险评估方法进行验证。结果 DEHP属于Cramer I类结构,其对应的TTC阈值为30μg/kg BW。我国居民的DEHP最大暴露量为4.06μg/kg BW,4个年龄组的最大暴露量为11.10μg/kg BW,分别占DEHP TTC阈值的13.5%和37.0%。按照DEHP的健康指导值———每日耐受摄入量(TDI)(50μg/kg BW)计算,全人群和4个年龄组的最大暴露量分别占TDI的8.1%和22.2%,两种方法的风险评估结果基本一致。结论 TTC决策树方法是一种有效的风险评估工具,可用于食品接触材料的优先筛选和初步评估。我国居民膳食DEHP的健康风险较低,不需要引起健康关注。     

紫外分光光度法测定饮用纯净水中邻苯二甲酸二己酯含量

目的：为建立饮用纯净水中的邻苯二甲酸二己酯含量的测定方法。方法：利用正己烷萃取饮用纯净水中的邻苯二甲酸二己酯,氮吹并用甲醇定容,建立紫外分光光度法对其进行含量测定,并对条件进行优化。结果：方法标准曲线方程为y＝1.5347x＋0.0266,线性相关系数为0.9970,该方法连续测定精密度为0.644%,重现性相对标准偏差为0.5742%,加标回收率为88.89%～97.73%。结论：建立紫外分光光度法测定瓶装饮用纯净水中邻苯二甲酸二己酯的方法,该方法简单快速,结果令人满意。     

Eleven phthalate esters and di(2-ethylhexyl) adipate in oneweek duplicate diet samples obtained from hospitals and their estimated daily intake

Plasticizers in duplicate diet samples obtained over 1 week were analysed in order to estimate daily intake. The phthalate esters were as follows: diethyl, dipropyl, dibutyl, dipentyl, dihexyl, butylbenzyl, dicyclohexyl, di(2-ethylhexyl), dioctyl, diisooctyl (mixture of isomers) and diisononyl (mixture). Di(2-ethylhexyl) adipate was also determined. Homogenized samples of composite meals were extracted with acetonitrile, lipids were removed by extraction into n-hexane and the acetonitrile layer was cleaned using FlorisilR and R Bondesil PSA dual layer column. Phthalates were determined by GC/MS (SIM). Phthalate recovery from the fortified food mixture by this method was 62.5-140.8%. Quality assurance as assessed by three laboratories indicated coefficient of variance in the levels of detected phthalates in same lot samples as below 10%. Detection limits were 0.1-23ng/g for each phthalate. One-week duplicate diet samples provided by three hospitals in three remote prefectures of Japan were analysed as individual meals. In all 63 samples, DEHP was present at the highest level among all phthalates in the range 10-4400ng/g. The intake of plasticizers estimated from all samples was 519 µ g DEHP/day, 86 µ g DEHA/day, 65 µ g DINP/day, and 4.7 µ g BBP/day. Calculated DEHP in 2-day samples out of 21 days exceeded EU TDI for a person of 50kg body weight (1850 µ g per day). Disposable PVC gloves used during the preparation of meals were suspected as the source of the high DEHP content. One-day intake of the other phthalates and DEHA was below 7% of TDI in all cases. High concentrations of DEHP (5990ng/g) was found in baby food used in quality assurance work. The source of contamination was the PVC-tube used during production and was effectively reduced by replacing the tube by one made of stainless steel.     

Migration of di(2-ethylhexyl) phthalate from polyvinyl chloride tubes used in preparation of foods

Three samples of polyvinyl chloride products for food use were examined for di(2-ethylhexyl) phthalate (DEHP) migration levels under the conditions described in the Japanese Food Sanitation Law. These samples were two kinds of tubes and one stretched film, containing 12 to 41% DEHP by weight. DEHP migration levels from them were very low, all below 0.1 ppm, into 3 kinds of food simulant; water, 4% acetic acid and 20% ethanol. However, high levels of DEHP migrated into n-heptane, 12 ppm from the stretched film sample and more than 800 ppm from the tube samples. Migration from the 2 tubes was higher than 150 ppm, the limit of residues after evaporation in containers and wraps. Though the limit of residues after evaporation is not set for equipment used in the preparation of foods, the tested tubes were considered to be unsuitable for uses in which they come into direct contact with oils, fats or oily foods.     

纸包装油墨中增塑剂向奶粉的迁移

纸包装油墨中含有有毒有害物质并可通过包装材料迁移进入内装食品从而危害人体健康。模拟实际印刷条件制作真实油墨迁移单元,研究纸张胶印油墨中4种主要增塑剂（3种邻苯二甲酸酯类增塑剂和近年流行的环保增塑剂乙酰基柠檬酸三丁酯）向奶粉的迁移,考察其在100、70、50、25 ℃的迁移行为,探讨增塑剂的性质及其在纸张中的分布等因素对迁移行为的影响。结果表明：4种增塑剂的最大迁移率在6.7%～67.8%之间。纸包装油墨中增塑剂的迁移防护性能还有待提高。     

A time-saving method for sealing Purdue Improved Crop Storage (PICS) bags

Purdue Improved Crop Storage (PICS) bags were designed to reduce grain storage losses on smallholder farms. The bag consists of three layers: two high-density polyethylene liners fitted inside a woven polypropylene bag. Recently, farmer groups, development relief programs, and government food security agencies have shown interest in PICS bags for large-scale use. PICS bags are conventionally closed by a twist-tie (TT) method, which involves twisting, folding, and tying the lip of each layer individually with a cord. This is not only time and labor intensive, but also may affect the integrity of the liners. We evaluated three new bag closure methods: i) inner liner rolled onto itself and middle liner fold-tied (IR), ii) both liners folded together and tied (FT), and iii) both liners folded and tied separately (FS), along with the conventional twist tie (TT) method. The time to close partially or fully filled 50 kg-capacity PICS bags filled with maize grain was assessed. Results showed that FT was the most time-saving method, reducing bag sealing time by >34% versus the usual TT method. The average internal oxygen levels reached <2% within a week in bags containing grain highly infested with Sitophilus zeamais, while it remained >5% levels for less-infested bags. In both cases, insect population growth was suppressed. Oxygen depletion rates among tying methods remained the same regardless of the closure method used. When large numbers of bags need to be closed, the time-saving FT method is a good alternative PICS sealing method over the conventional twist-tie approach.