食品包装材料中邻苯二甲酸酯类增塑剂迁移量的测定

建立了一种食品包装材料中邻苯二甲酸酯类(PAEs)增塑剂迁移量的检测方法。以正己烷为萃取溶剂对食品包装材料模拟液中17种PAEs进行提取,然后采用气相色谱-质谱联用法(GC-MS)进行检测。结果表明:17种PAEs的分离较好,方法检出限为0.14~0.30 mg/kg,线性范围0.5~8.0 mg/L,相关系数大于0.996,相对标准偏差(RSD)为2.2%~4.8%,回收率为95.0%~116.0%。该方法操作简便、准确、分离效果好,可同时检测食品包装材料中17种PAEs类增塑剂的迁移量。     

GC-MS法测定聚乙烯塑料袋中的邻苯二甲酸酯

建立了一种检测聚乙烯(PE)塑料袋中邻苯二甲酸酯(PAEs)类物质残留含量的方法。以正己烷为萃取溶剂,利用超声萃取法对样品中的PAEs进行了提取,随后采用气相色谱-质谱联用法(GC-MS)对其进行了定性、定量的检测。结果表明:利用该方法所得样品中PAEs的加标(16种PAEs混标)回收率分别在80.06%¹28.47%之间,检出限在0.057 5128.47%之间,检出限在0.057 5⁰.907 6 mg/kg之间,相对标准偏差(RSD)在6.92%0.907 6 mg/kg之间,相对标准偏差(RSD)在6.92%¹0.88%之间。该方法操作简便,重现性好。     

气相色谱-质谱法同时测定橡塑材料中18种邻苯二甲酸酯类增塑剂

对塑料和橡胶分别以正己烷和乙醚为提取溶剂,通过自动索氏提取,并根据需要将提取液经硅胶固相萃取小柱富集净化,用气相色谱-质谱法(GC-MS)的分段选择离子监测(SIM)对两种材料中18种邻苯二甲酸酯(PAEs)进行检测。该方法具有良好线性,相关系数R均大于0.999,检测限在6.03～727.67μg/kg之间,塑料材料和橡胶材料18种PAEs的平均回收率分别在80.02%～114.33%和77.64%～113.04%,RSD值分别在1.03%～7.39%和1.69%～8.40%。该方法具有操作简单、灵敏度高、重现性好,能同时检测18种PAEs的特点,进一步满足了国内外在橡塑材料中邻苯二甲酸酯的检测需求。     

新型微波辅助-基质分散固相萃取技术结合HPLC测定土壤中塑化剂

建立基于低共熔溶剂(DESs)的微波辅助-基质分散固相萃取技术结合高效液相色谱法(HPLC)测定土壤中邻苯二甲酸酯类塑化剂(PAEs)的方法。采用在土壤样品中分别加入不同的分散剂和DES研磨分散的方法进行目标物提取,并将混合物经微波萃取后装入固相萃取小柱并用正己烷洗脱,提取液采用高效液相色谱法(HPLC)检测PAEs。结果表明：在优化实验条件下,5种PAEs的线性范围分别为0.1～500、0.1～500、0.1～500、0.1～500、0.1～1 000μg/mL,检出限分别为0.01、0.01、0.01、0.01、0.02μg/mL,DMP、DEP、DBP、DPP、DCHP的加标回收率分别为93.41%、93.43%、93.71%、97.98%、97.58%。此方法操作快速、简便、灵敏度高,结果令人满意,可适用于土壤中PAEs的定量检测。     

几种常用塑料给水管道邻苯二甲酸酯检测方法研究

通过气相色谱-质谱联用法(GC-MS)对几种塑料给水管道中邻苯二甲酸酯(PAEs)的含量进行了检测,其中着重探讨了不同前处理及萃取方式对检测结果及检测效率的影响。结果表明:对样品进行研磨处理有利于提高检出精度;3种萃取方式(超声波萃取、搅拌萃取、索氏萃取)的萃取效率基本等同,均能满足快速检测的要求。对于3种常见的塑料给水管道——聚氯乙烯(PVC)管、聚乙烯(PE)管、无规共聚聚丙烯(PPR)管,仅PVC管及PE管中含有PAEs。     

用索氏提取-气相色谱法测定PVC管材中的邻苯二甲酸酯类增塑剂

建立了索氏提取-气相色谱法测定聚氯乙烯(PVC)等管材中6种国家限量邻苯二甲酸酯(PAEs)类增塑剂的方法。采用索氏提取作为前处理提取手段,通过正交试验对样品中PAEs类增塑剂的提取条件进行系统优化。结果表明:在一定范围内,该方法具有良好线性关系,相关系数在0.997~0.999之间,检测限为0.15~0.60 mg/kg,平均回收率84.2%~109%,相对标准偏差为1.33%~8.60%。方法简单高效,具有良好的重现性和灵敏度,适用于PVC等管材中PAEs类增塑剂的分析检测。     

超声萃取-气质联用法测定食品包装中6种PAEs

建立了超声萃取-气质联用法测定食品塑料包装中6种PAEs(DMP、DEP、DBP、DPP、DHP和DEHP),并对样品前处理和色谱条件进行了优化。结果表明:20℃或室温条件下,以正己烷为提取剂,超声萃取30min时,6种物质的提取效果较好;在0.5mg/L~8.0mg/L线性范围内,6种物质的相关系数均在0.999以上,定性检出限在1.85μg/L~3.75μg/L之间,定量检测限在6.16μg/L~12.5μg/L之间;回收率为85.9%~108%,相对标准偏差(RSD)为1.22%~3.59%。因此,所建方法简便准确、快速有效,为食品塑料包装中6种PAEs的检测提供参考。     

GC-MS法同时测定塑料中十六种微量PAEs

建立了同时测定塑料中16种微量邻苯二甲酸酯类化合物(PAEs)的气相色谱-质谱(GC-MS)分析方法。对样品前处理方法和色谱条件进行了优化,采用乙酸乙酯作为溶剂,使用快速溶剂萃取仪对塑料样品中的PAEs进行萃取。经优化后该方法线性范围宽,线性关系好,对16种PAEs的检出限达到0.5~1.9μg/g。对整个方法的精密度和准确度进行了衡量,16种PAEs在2个添加水平时的平均回收率为90.2%~111.0%,相对标准偏差(n=5)为2.1%~10.8%。对不同品种的塑料样品进行了检测,检出2~6种不同含量的PAEs。     

化妆品塑料包装材料中16种邻苯二甲酸酯的测定

为了建立化妆品塑料包装材料中邻苯二甲酸酯(PAEs)的测定方法,通过设计正交试验,优化超声振荡萃取的条件,并通过气相色谱-质谱联用仪进行测定。结果表明:16种PAEs在线性范围内的相关系数均大于0.996,方法检出限0.157~0.928 mg/L,加标回收率在87.4%~108.3%范围内,RSD(n=6)均小于7.0%。聚对苯二甲酸乙二醇酯(PET)、聚丙烯(PP)、丙烯腈-丁二烯-苯乙烯(ABS)、聚苯乙烯(PS)中PAEs的检出率达到82.6%。该方法操作简单,高效准确,可以检测不同化妆品塑料包装的PAEs。     

液-液萃取法提取水环境中PAEs污染物的萃取剂筛选

选取不同有机溶剂作为萃取剂提取水环境中邻苯二甲酸酯(PAEs)污染物,以筛选合适萃取剂。结果表明,正己烷和乙酸乙酯1∶1混合液对5种PAEs单品的回收率和可操作性均较优,适宜作为水环境PAEs污染物含量分析检测时的萃取剂。此外,乙酸乙酯溶剂对环境中的邻苯二甲酸丁基苄基酯(BBP)回收率较高,可达到97. 57%;石油醚和乙酸乙酯1∶1混合溶液对BBP和邻苯二甲酸二甲酯(DMP)回收率可以达到94. 12%和92. 62%;二氯甲烷对邻苯二甲酸二正丁酯(DBP)的回收率可以达到了94. 21%。     

开放式超声微波协同萃取测定PVC塑料中邻苯二甲酸酯类增塑剂研究

概述了邻苯二甲酸酯类(PAEs)作为聚氯乙烯(PVC)增塑剂的应用、危害,说明了PAEs的理化性质,详细归纳了超声波、微波、超声.微波协同萃取技术的应用及PAEs分析测定方法.通过优化超声波、开放式微波和超声.微波等方式萃取PVC塑料样品中的PAEs的萃取条件,比较了3种不同萃取方式的萃取效率.结果表明,超声.微波协同萃取是比较理想的萃取方式.利用该方法对2种实际塑料样品中PAEs的萃取和分析,成功地定量测定了PVC塑料样品中DEHP、DINP和DBP等邻苯二甲酸酯类增塑剂的含量.该法可用于塑料制品中各类邻苯二甲酸酯类增塑剂的快速萃取和分析.     

湘江水中邻苯二甲酸酯类环境激素的研究

采用分散液液微萃取-高效液相色谱法测定湘江株洲段水体中邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二正丁酯(DBP)和邻苯二甲酸丁苄酯(BBP),利用正交实验优化了萃取条件,分析其污染水平分布,并进行生态风险评价。结果表明:4种邻苯二甲酸酯类物质普遍检出,∑PAEs的浓度范围为22.39～27.4μg/L,其中DBP为主要污染物。利用商值法对PAEs进行生态风险评价,各种物质均存在潜在生态风险。     

Ionic liquid enhanced magnetic solid-phase extraction of phthalate esters in food samples with oleic acid coated-Fe3O4 nanoparticles prior to HPLC

A novel method based on ionic liquid enhanced magnetic solid-phase extraction (MSPE) coupled with high-performance liquid chromatography (HPLC) for the separation/analysis of phthalate esters (PAEs) in food samples was established. 1-hexyl-3-methylimidazoliu-hexafluorophosphate ([C₆MIM][PF₆]) was used to coat oleic acid Fe₃O₄ nanoparticles with core–shell structures to prepare MSPE agents (Fe₃O₄@OA@IL). The main parameters affecting the extraction efficiency of PAEs were studied. Under the optimal conditions, the calibration curves were linear in the range of 5–5000 ng mL^?1 (R² = 0.9972–0.9998) of four PAEs. The limit of detections (LODs) and relative standard deviations (RSDs, n = 5) of the method were 1.27–2.95 ng mL^?1 and 3.9–5.3%, respectively.     

GC-MS法同时测定塑料玩具中22种邻苯二甲酸酯增塑剂

建立了气相色谱-质(谱GC-MS)法,采用分段选择离子监(测SIM)模式,同时测定了塑料玩具中22种邻苯二甲酸酯(类PAEs)增塑剂的含量。结果表明:该方法具有良好的线性关系,相关系数均大于0.999,检测限在1.28~128.91mg/kg之间,平均回收率70.83%~107.95%,相对标准偏差3.61%~9.79%。该方法操作简单,灵敏度高重,现性好能,满足塑料玩具中PAEs含量的检测需求。     

Biodegradation of Di-n-Butyl Phthalate by a Newly Isolated Halotolerant Sphingobium sp.

A Gram-negative strain (TJ) capable of growing aerobically on mixed phthalate esters (PAEs) as the sole carbon and energy source was isolated from the Haihe estuary, Tianjin, China. It was identified as belonging to the Sphingobium genus on the basis of morphological and physiological characteristics and 16S rRNA and gyrb gene sequencing. The batch tests for biodegradation of di-n-butyl phthalate (DBP) by the Sphingobium sp. TJ showed that the optimum conditions were 30 °C, pH 7.0, and the absence of NaCl. Stain TJ could tolerate up to 4% NaCl in minimal salt medium supplemented with DBP, although the DBP degradation rates slowed as NaCl concentration increased. In addition, substrate tests showed that strain TJ could utilize shorter side-chained PAEs, such as dimethyl phthalate and diethyl phthalate, but could not metabolize long-chained PAEs, such as di-n-octyl phthalate, diisooctyl phthalate, and di-(2-ethyl-hexyl) phthalate. To our knowledge, this is the first report on the biodegradation characteristics of DBP by a member of the Sphingobium genus.     

城市给水厂应对原水发生邻苯二甲酸酯污染的处理技术及处理效能

城市水源水邻苯二甲酸酯(PAEs)污染对饮用水水质安全产生了威胁。综述了国内地表水(包括城市水源水)和给水厂处理出水中PAEs的污染情况,提出粉末炭(PAC)吸附与混凝沉淀联用技术(以下简称联用技术)是适合国内目前大多数水厂实情的可以有效应对水源水发生PAEs污染的水处理技术。开展了联用技术对原水中邻苯二甲酸二(2-乙基己基)酯(DEHP)的去除效能的实验研究。结果表明,联用技术可以有效地去除原水中DEHP,处理出水浊度是影响DEHP去除效果的重要因素,PAC理化特征对联用技术去除原水中DE-HP效果的影响不大。最后基于小试实验结果给出了不同污染水平下联用技术中PAC的建议投量,为实际生产提供了技术参考。     

Transformation of phthalic acid diesters in an anaerobic/anoxic/oxic leachate treatment process

Transformations of di-n-butyl phthalate(DBP) and di(2-ethylhexyl) phthalate(DEHP) have been investigated in anaerobic/anoxic/oxic(A/A/O) leachate treatment processes. Although the DBP removal processes are different when the DBP initial concentration is different, the overall system DBP removal efficiencies are high(N 94%).DEHP is much more difficult to remove than DBP. The removal efficiency of DEHP is approximately 75%–78%.The results of mass balance calculations indicate that approximately 33.7%–50.7% of the DBP is degraded by the activated sludge, 48.9%–64.9% accumulates in the system, and 0.4%–1.4% is contained in the final effluent. Approximately 15.0%–19.0% of the DEHP is degraded by activated microcosms, 75.8%–79.0% accumulates in the system, and 5.2%–6.0% is contained in the final effluent. Biodegradation and adsorption to the activated sludge are the main mechanisms for DBP removal and adsorption to the activated sludge is the main mechanism for DEHP removal. The different removal mechanisms of the two PAEs may be related to their different molecular structures. However, PAEs are not really removed when they adsorb onto the sludge. Therefore, methods for decreasing PAEs adsorption and increasing the biodegradation efficiencies of the leachate treatment processes should be further investigated.     

高效液相色谱法测定环境样品中的酞酸酯

研究了高效液相色谱法测定环境样品中酞酸酯含量的色谱分离条件,采用薄层色谱预分离的方法减少杂质峰对样品的干扰,对部分月份环境样品中的酞酸酯富集程度进行了检测。     

An alternative to DEHP plasticized polyvinyl chloride in chemotherapy drug delivery systems

Medical plastic selection has recently been challenged with the development and approval of a new chemotherapy drug that, because of the carrier solution used, causes extraction of di-2-ethylhexyl phthalate (DEHP) plasticizer from commonly used polyvinyl chloride (PVC). There is much discussion as to whether or not this extraction is a problem. However, in an effort to comply with the recommendations of the drug manufacturer, many device companies are in the process of converting their devices from DEHP plasticized tubing to tubing made with non-phthalate plasticizer. This paper describes the effort made to both understand and comply with the recommendations made by the drug manufacturer. The testing confirms effective reduction of the phthalate plasticizer extraction.