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1.
本实验建立了超声提取-气相色谱-串联质谱法(polycyclic aromatic hydrocarbons, PAHs)测定煎烤鱿鱼中16种多环芳烃的分析方法。考察了提取试剂配比、提取试剂用量、提取温度等对回收率的影响,确定了最佳的提取和检测方法:5.00 g样品冷冻干燥后经25 mL正己烷30 ℃超声提取20 min,复提一次,经碱性氧化铝-中性硅胶复合固相萃取柱净化后,采用气相色谱-串联质谱法测定,多环芳烃氘代内标法定量。在此实验条件下,16种目标物在1~100 ng/mL范围内呈良好线性关系,线性相关系数(r)不低于0.9994,检出限为0.09~0.52 μg/kg,定量限为0.21~1.21 μg/kg。在1、2、20 μg/kg 3个加标水平下回收率分别为73.98%~128.17%、73.21%~133.24%、76.35%~133.68%,相对标准偏差(RSD,n=6)分别为1.32%~2.98%、0.93%~2.47%、1.08%~2.87%。在实际样品检测应用中,6个样品均有不同程度的多环芳烃检出,单一组分检出范围从0~48.65 μg/kg不等。结果表明,该方法选择性好,可用于煎烤鱿鱼中多环芳烃的检测,也可应用于其他类似的加工水产品中多环芳烃的提取与检测。  相似文献   

2.
建立北京烤鸭鸭皮中16 种多环芳烃(polycyclic aromatic hydrocarbons,PAHs)的凝胶渗透色谱(gel permeation chromatography,GPC)净化-气相色谱-质谱(gas chromatography-mass spectrometry,GC-MS)检 测分析方法。匀浆后的烤鸭鸭皮样品经乙酸乙酯超声提取20 min,采用GPC净化,GC-MS进行检测。结果表 明:16 种PAHs在1~100 μg/L质量浓度范围内线性关系良好(R2>0.996),检出限为0.08~0.39 μg/kg,定量 限为0.25~1.29 μg/kg;在1、5、10 μg/kg添加水平下,16 种PAHs的回收率为66.2%~108.3%,相对标准偏差为 0.7%~13.5%(n=6),满足分析要求;采用该方法对购自超市的北京烤鸭进行检测,烤鸭鸭皮样品中均未检出苯 并(a)芘,苯并(a)芘、苯并(a)蒽、苯并(b)荧蒽和?总含量也未超过欧盟限量标准(12.0 μg/kg)。  相似文献   

3.
建立了大米中16种多环芳烃残留的气相色谱-质谱(GC-MS)检测方法。样品中的多环芳烃经乙腈提取,改进基质固相分散技术(QuEChERS)净化后,进行GC-MS测定,同位素内标法定量。方法的样品加标回收率和精密度分别为69.1%~96.9%和8.2%~12.7%。多环芳烃的方法检测限为0.6~3.2μg/kg。  相似文献   

4.
本文建立了一种气相色谱质谱联用法定量测定饲料原料中16种多环芳烃的方法。以苊-D10、?-D12和苯并(a)芘-D12为内标物,对饲料原料中的多环芳烃提取、净化和定量方法进行优化。结果表明,在2~1000 ng/mL范围内,16 种多环芳烃峰面积与内标物峰面积比值均与质量浓度比值呈良好线性关系,相关系数均大于0.999;检出限和定量限分别为 0.6 μg/kg~1.2 μg/kg、1.8 μg/kg~3.6 μg/kg;在2 μg/kg、5 μg/kg、20 μg/kg三个加标水平下,回收率在 75.6%~94.8%之间,相对标准偏差在0.8%~11.9%之间。该方法净化效果好、灵敏度高、重复性好,具有较强的复杂基质抗干扰能力,可用于批量饲料原料样品中的多环芳烃的定量测定。  相似文献   

5.
摘 要: 目的 优化辣条基质中多环芳烃(polycyclic aromatic hydrocarbons, PAHs)的检测方法。方法 采用乙腈提取-QuEChERS净化处理的方式, 通过提取溶剂种类和用量的优化, 建立高效液相色谱-二极管阵列检测器-荧光检测器联用检测辣条中16种多环芳烃的快速分析方法。结果 采用空白基质提取液配制标准曲线溶液, 16种多环芳烃在20~500 ng/mL的范围内线性良好, 各目标物R2范围在0.9989~1.000之间, 检出限为0.08~4.00 μg/kg, 定量限为0.3~15 μg/kg实际样品测试中, 20、40和200 μg/kg 3个水平加标回收率为73.09%~106.86%, 相对标准偏差为0.73%~4.48%。结论 该方法灵敏度好、回收率高、精密度高, 适用于辣条中16种多环芳烃的分析检测。  相似文献   

6.
目的 建立植物油中多环芳烃的分子印迹固相萃取-高效液相色谱快速测定方法。方法 采用正己烷溶解植物油样品, 将样品上样于活化和平衡后的分子印迹固相萃取小柱, 正己烷淋洗, 二氯甲烷洗脱, 氮吹至近干后, 1 mL正己烷定容, 0.22 μm亲水系PTFE滤膜过滤, 高效液相色谱法荧光检测器测定, 保留时间定性, 色谱峰面积定量。结果 多环芳烃在1~100 ng/mL浓度范围内, 峰面积呈良好线性, 线性相关系数均达到0.999以上。多环芳烃在5.0、20.0、50.0 μg/kg 3个不同添加水平的回收率为76.0%~103.6%, 相对标准偏差(relative standard deviation, RSD)均小于10%。结论 该方法具有简便、快速、灵敏高、准确度好等优点, 可满足植物油中多环芳烃的定量分析。  相似文献   

7.
刘冰  霍鲁格 《现代食品科技》2013,29(6):1395-1399
本文建立了鱼肉中16种多环芳烃的气相色谱-三重四级杆串联质谱(GC-QqQ-MS/MS)的检测方法。样品通过正己烷/二氯甲烷(1/1,V/V)超声波提取,经弗罗里硅土柱净化后,采用TR-5MS毛细管柱分离,以电子轰击(EI)电离、选择反应检测模式(SRM)检测。讨论了洗脱溶剂对净化效果的影响,以及基质效应对各种多环芳烃测定的影响。通过基质匹配标准曲线进行定量,16种多环芳烃在0.4 μg/kg到50 μg/kg范围内相性关系良好,线性相关系数为0.9865~0.9999。方法检出限从0.024 μg/kg到0.06 μg/kg,方法的定量限从0.08 μg/kg到0.2 μg/kg。16种多环芳烃在5、10、50 μg/kg加标水平下的回收率为68.5%到106.3%,相对标准偏差为0.4%到17.8%,对常见的鱼类样品进行测定,结果令人满意。  相似文献   

8.
目的 建立了气相色谱串联质谱法(gas chromatography-tandem mass spectrometry, GC-MS/MS)测定中华绒鳌蟹中16种多环芳烃(pycyclic aromatic hydrocarbons, PAHs)的分析方法。方法 中华绒螯蟹样品与硅藻土研末混匀后经快速溶剂萃取仪(accelerated solvent extraction, ASE)提取, 使用凝胶渗透色谱(gel permeation chromatography, GPC)净化, 全自动浓缩仪在线浓缩后,在多级离子反应监测(multistage ion reaction monitoring, MRM)模式下分析, 采用同位素内标法进行定量。结果 16种多环芳烃(PAHs)在1~100 ng/mL范围内,线性关系良好, 相关系数(r)≥0.995。定量限在0.3~0.5μg/kg, 在1.0、2.0、10.0 μg/kg三个加标水平下, 16种PAHs的平均回收率为80.3%~105.4% , 相对标准偏差(relative standard deviation, RSD)小于10.3%。结论 该方法自动化程度高、准确、稳定、可靠, 可用于测定中华绒螯蟹中16种PAHs的残留量。  相似文献   

9.
目的 建立固相微萃取-气相色谱-质谱联用仪测定醇食品模拟液中16种多环芳烃的分析方法。方法 优化了萃取方式、萃取温度、萃取时间、解吸时间和振荡速率等萃取条件, 样品采用气相色谱-质谱联用仪(gas chromatography-mass spectrometry, GC-MS)总离子流和选择离子模式进行定性定量测定。结果 16种多环芳烃在0.01~10 ?g/L范围内线性良好, R2大于0.99。在0.1、0.5、1.0 μg/L 3个添加水平下, 16种多环芳烃的平均回收率为76.52%?119.8%, 相对标准偏差为0.99%?15.93%。结论 该方法操作简便、灵敏度高、准确度好, 能够满足醇食品模拟物中多环芳烃化合物的检测要求。  相似文献   

10.
为稳定可靠地分析油茶籽油中多环芳烃,建立了分子印迹固相萃取-气相色谱-串联质谱测定油茶籽油中16种多环芳烃方法。样品经正己烷溶解后,分别采用反相固相萃取HLB小柱、弗罗里硅土小柱和分子印迹固相萃取小柱对16种多环芳烃进行净化。以回收率和基质效应为考察指标评估3种固相萃取柱的净化,在此基础上,对净化液进行低温低速氮吹浓缩,多反应监测扫描模式下进行气相色谱-串联质谱检测,外标法定量。结果表明:分子印迹固相萃取小柱对16种多环芳烃的净化效果最佳;16种多环芳烃在质量浓度1~50 μg/L范围内线性关系良好(R2≥0.995 1),检出限为0.01~ 0.20 μg/kg,在2、10 μg/kg和20 μg/kg加标水平下的回收率为71.5%~116.3%,相对标准偏差为1.5%~13.8%。该方法具有灵敏度高、检出限低、重复性好等特点,适用于油茶籽油中16种多环烃的测定。  相似文献   

11.
A 9% whey protein (WP) isolate solution at pH 7.0 was heat-denatured at 80°C for 30 min. Size-exclusion HPLC showed that native WP formed soluble aggregates after heat-treatment. Additions of CaCl2 (10–40 mM), NaCl (50–400 mM) or glucono-delta-lactone (GDL, 0.4–2.0%, w/v) or hydrolysis by a protease from Bacillus licheniformis caused gelation of the denatured solution at 45°C. Textural parameters, hardness, adhesiveness, and cohesiveness of the gels so formed changed markedly with concentration of added salts or pH by added GDL. Maximum gel hardness occurred at 200 mM NaCl or pH 4.7. Increasing CaCl2 concentration continuously increased gel hardness. Generally, GDL-induced gels were harder than salt-induced gels, and much harder than the protease-induced gel.  相似文献   

12.
The levels of bisphenol-F-diglycidyl ether (BFDGE) were quantified as part of a European survey on the migration of residues of epoxy resins into oil from canned fish. The contents of BFDGE in cans, lids and fish collected from all 15 Member States of the European Union and Switzerland were analysed in 382 samples. Cans and lids were separately extracted with acetonitrile. The extraction from fish was carried out with hexane followed by re-extraction with acetonitrile. The analysis was performed by reverse phase HPL C with fluorescence detection. BFDGE could be detected in 12% of the fish, 24% of the cans and 18% of the lids. Only 3% of the fish contained BFDGE in concentrations considerably above 1mg/kg. In addition to the presented data, a comparison was made with the levels of BADGE (bisphenol-A-diglycidyl ether)analysed in the same products in the context of a previous study.  相似文献   

13.
Microgels are ‘soft’ microscopic cross-linked polymeric particles that are being increasingly exploited in a variety of industries for rheology control, encapsulation and targeted delivery. They are valued because of the ability to tune their functionality to address specific applications in oil recovery, coatings, drug delivery, cosmetics, personal care and foods. Food microgels are typically biopolymer hydrogels in the form of microspheres, nanospheres (also called nanogels), spheroids and fibres. The utilisation of engineered microgels in foods has so far been limited, despite their great potential to address several needs in the food industry, including: satiety control, encapsulation of phytonutrients and prebiotics, texture control for healthier food formulations (e.g. reduced fat products), and targeting delivery to specific areas in the digestive tract. We review the scientific and patent literature on the utilisation and manufacturing methods for producing microgels with an emphasis on micro-hydrogels for food applications.  相似文献   

14.
Joubert and Burns prepared a large number of fractions from the high-sulphur proteins of wool and estimated their molecular weights and amino-acid compositions. Their data have been re-examined in order to look for statistically significant interrelations between amino acids and between the proportion of various amino acids and molecular weight. Statistical analysis of the data is also used to examine the credibility of some hypotheses concerning the mechanism of keratin biosynthesis and to provide further evidence for the existence of families of proteins within the high-sulphur fractions of wool.  相似文献   

15.
The European Commission's, Quality of Life Research Programme, Key Action 1—Health, Food & Nutrition is mission-oriented and aims, amongst other things, at providing a healthy, safe and high-quality food supply leading to reinforced consumer confidence in the safety of European food. Its objectives also include the enhancing of the competitiveness of the European food supply. Key Action 1 is currently supporting a number of different types of European collaborative projects in the area of risk analysis. The objectives of these projects range from the development and validation of prevention strategies including the reduction of consumers risks; development and validation of new modelling approaches; harmonization of risk assessment principles, methodologies, and terminology; standardization of methods and systems used for the safety evaluation of transgenic food; providing of tools for the evaluation of human viral contamination of shellfish and quality control; new methodologies for assessing the potential of unintended effects of genetically modified (genetically modified) foods; development of a risk assessment model for Cryptosporidium parvum related to the food and water industries; to the development of a communication platform for genetically modified organism, producers, retailers, regulatory authorities and consumer groups to improve safety assessment procedures, risk management strategies and risk communication; development and validation of new methods for safety testing of transgenic food; evaluation of the safety and efficacy of iron supplementation in pregnant women; evaluation of the potential cancer-preventing activity of pro- and pre-biotic ('synbiotic') combinations in human volunteers. An overview of these projects is presented here.  相似文献   

16.
<正>We are pleased to announce the launch of a new international peer-reviewed journal-Food Science and Human Wellness,ISSN 2213-4530,which is an open access journal,produced and hosted by Elsevier B.V.on behalf of Beijing Academy of Food Sciences.Food Science and Human Wellness is an international peer-reviewed English journal that provides a forum for the dissemination of  相似文献   

17.
《印刷工业》2014,(9):94-95
In the 2014 China(Shanghai)International Printing Week,Director Wang Yanbin released the latest data about development of Chinese printing industry in 2013.According to statistics,in 2013,the total output value of Chinese printing industry exceeded 1trillion Yuan for the first time,reaching 1.03985 trillion Yuan.There were 105,000 printing enterprises in China,employees were 3.415 million.The total asset was 1.06247 trillion Yuan;  相似文献   

18.
正On December 2nd,2013,the State Council issued the notification of"Directory of Government Approved Investment Projects(2013 Edition)"(hereafter referred to as"notification").It is pointed out in the"notification"that in order to further deepen reforms in investment systems and administrative examination and approval systems,simplify administrative procedures and delegate powers to lower levels,earnestly  相似文献   

19.
正Among the 1600 exhibitors who take apart in the ITMA ASIA+CITME2014 2/3 are Chinese manufactures.If the numerous figures failed to attract your attention,the increase of quality should draw your focus.To adopt the demand of developing textile machine market,domestic textile machinery enterprises now follow the slogan of"technology drives development"to enhance product competitiveness.Our domestic sellers will showcase product ranging from spinning,weaving,dyeing and printing,  相似文献   

20.
《造纸信息》2014,(8):99-100
On December 24th, 2013, the meeting on the selection of top 10 news of China's paper industry 2013 sponsored by 〈China Paper Newsletters〉 was held in Beijing. The yearly selection of the top l0 news, which began in 2000, has become a brand activity widely recognized in the industry thanks to the support from the authorities at all levels and public participation.  相似文献   

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