反相高效液相色谱-荧光法同时测定食品中叔丁基对苯二酚和叔丁基羟基茴香醚的含量

1 引言 油溶性抗氧化剂叔丁基对苯二酚(tert-butyl hydroquinone,TBHQ)、叔丁基羟基茴香醚(butylated hydroxyanisole,BHA)和2,6-二叔丁基对甲酚(butylated hydroxytoluene,BHT)是目前最常用的化学合成抗氧化剂,能够有效阻止或延迟油脂氧化变质.     

离子液体双水相萃取-高效液相色谱法测定香精香料中的抗氧化剂

建立了香精香料中没食子酸丙酯(PG)、特丁基对苯二酚(TBHQ)、叔丁基对羟基茴香醚(BHA)和2,6-二叔丁基对甲酚(BHT)四种抗氧化剂的高效液相色谱检测方法。香精香料样品经离子液体双水相前处理,用高效液相色谱-二极管阵列检测法(HPLC-DAD)测定。结果表明,在0.5～100μg/mL浓度范围内,四种抗氧化剂的色谱峰面积均与其浓度呈线性关系,相关系数r≥0.9990,检出限分别为3.0、7.1、5.1和9.7ng/mL,回收率为85%～97%,相对标准偏差为1.2%～6.7%。     

双(2,6-二叔丁基-4-甲基苯基)季戊四醇二磷酸酯的合成

以季戊四醇(1),三氯化磷(2)和2,6-二叔丁基对甲酚(3)为原料,三乙胺为催化剂和缚酸剂,经一锅法合成了双(2,6-二叔丁基-4-甲基苯基)季戊四醇二磷酸酯(PEP-36),其结构经1H NMR,13C NMR,IR和ESI-MS确证。采用正交试验对反应条件进行了优化。在最佳反应最佳条件[三乙胺为催化剂和缚酸剂,1 100 mmol,n(1)∶n(2)∶n(3)=1.0∶2.4∶2.4,于110℃反应12 h后于125℃反应12 h]下,PEP-36的收率70.2%,纯度99.07%。     

中空纤维膜液相微萃取技术／气相色谱-质谱法对食品中防腐剂与抗氧化剂的测定

将中空纤维膜液相微萃取技术与气相色谱-离子阱质谱联用,测定食品中的4种防腐剂(对羟基苯甲酸甲酯(MP)、对羟基苯甲酸乙酯(EP)、对羟基苯甲酸丙酯(PP)及对羟基苯甲酸丁酯(BP))和3种抗氧化剂(叔丁基-4-羟基苯甲醚(BHA)、叔丁基苯二酸(TBHQ)、2,6-二叔丁基对甲酚(BHT)).优化的萃取条件:以15%(质量分数)Na2SO4的盐溶液为稀释溶剂,5 μL甲苯为萃取溶剂,搅拌速率为1 200 r/min,萃取时间为15 min.该方法的线性范围为0.4 ～80 mg/kg,检出限为0.002 ～8.0 μg/kg,加标回收率为94% ～115%,相对标准偏差为4.38% ～9.34%.     

聚乙烯塑料包装材料中4种抗氧化剂向脂肪食品模拟物迁移的研究

本文基于超高效液相色谱建立了一种脂肪食品模拟物异辛烷中抗氧化剂叔丁基对羟基茴香醚(BHA)、2,6-二叔丁基对甲酚(BHT)、四[甲基-β-(3,5-二叔丁基-4-羟基苯基)丙酸酯]季戊四醇酯(Irganox1010)以及β-(4-羟基-3,5-二叔丁基苯基)丙酸正十八酯(Irganox1076)的提取检测方法,加标回收率在78.0%～108.7%之间,相对标准偏差(RSD)在4.0%～13.7%之间。研究了聚乙烯(PE)膜中抗氧化剂向异辛烷的迁移,讨论了温度及时间对迁移的影响,并根据迁移数据进行了初步的数学模型的建立,对实验值与数值模拟结果计算值作了对比分析。     

酚类在芳烃溶剂中的缔合溶液热力学

用凝固点降低法测量了对甲酚、间甲酚、邻甲酚、2,4-二甲酚、2,6-二甲酚以及对甲酚+间甲酚、对甲酚+邻甲酚、间甲酚+邻甲酚、2,4-二甲酚+2,6-二甲酚的1:1摩尔比混合物等为溶质, 溶剂为苯或对二甲苯的活度系数, 用Wiehe-Bagley型的连续缔合模型对数据进行了处理, 得到了各种酚的自缔合常效K_A. 在同一溶剂中, K_A依下列顺序减小: 对甲酚>间甲酚>邻甲酚; 2,4-二甲酚>2,6-二甲酚. 各混合酚的表观K_A 介于两种纯酚的K_A之间.     

超高效液相色谱-质谱法测定油脂中的10种抗氧化剂

对油脂中的没食子酸丙酯(PG),没食子酸辛酯(OG)、2,4,5-三羟基苯丁酮(THBP)、叔丁基对苯二酚(TBHQ)、叔丁基对羟基茴香醚(BHA)、2,6-二叔丁基对甲酚(BHT)、没食子酸十二酯(DG)、正二氢愈创酸(NDGA)、2,6-二叔丁基-4-羟甲基苯酚(HMBP)和没食子酸异戊酯(IAG)10种抗氧化剂进行了超高效液相色谱-质谱法(UPLC/MS)测定的系统研究,建立了一种简单、快速、准确测定油脂中10种抗氧化剂的测定方法。对样品中提取溶剂和提取时间的选择以及相关线性、精密度、回收率作了考察和实验。结果表明,本方法能有效提取油脂样品中的这10种抗氧化剂,并对其进行UPLC/MS分离和测定。10种抗氧化剂的平均回收率为92.56%～102.5%(n=6),相对标准偏差为0.68%～5.12%(n=6),检出限为2～10μg/L。     

高效液相色谱法测定食用植物油中5种抗氧化剂的含量

提出了高效液相色谱法测定食用植物油中没食子酸丙酯、特丁基对苯二酚、叔丁基羟基茴香醚、没食子酸辛酯和2,6-二叔丁基对羟基甲酚等5种抗氧化剂的方法。样品(1.000g)用甲醇5mL)提取2次,涡旋振荡10min,取上清液在4℃冷藏,使残留脂肪析出。取其上清液浓缩后用甲醇定容为10 mL,取5μL进样用高效液相色谱法进行测定。ZORBAX SB-C_(18)色谱柱及不同比例混合的甲醇(A)和乙酸-水(1+99)(B)的混合液作为流动相进行梯度淋洗分离,柱温为30℃,流量为1.0mL·min~(-1),检测波长为280 nm。结果表明:5种抗氧化剂的检出限(3S/N)依次为0.10,0.34,0.32,0.14,0.57mg·kg~(-1)。在3个浓度水平上(200,500,1000mg·kg~(-1))对方法做回收试验,测得回收率在90.5%～102.0%之间,相对标准偏差(n=6)在0.02%～1.35%之间。     

反相高效液相色谱-质谱法测定喷气燃料中抗氧剂含量

分析喷气燃料中抗氧剂的真实含量对于研究和控制喷气燃料贮存的安全性具有重要意义。国外Cunningham等[1]用高效液相色谱 紫外检测器分析抗氧剂,国内目前普遍采用正相色谱,即以正己烷为流动相、用硅胶色谱柱和紫外检测器,直接测定喷气燃料中抗氧剂2,6 二叔丁基对甲酚的含量     

频率位移测定及焓变的计算 Ⅰ.关于酚类与含氧或氮碱的加成物

用付里叶变换红外光谱技术测定了酚,4-叔丁基酚,2-叔丁基酚,3,5-二叔丁基酚,2,6-二叔丁基酚与一些含氧或氮的路易士碱组成的19对酸碱体系中OH的频率位移△νOH。根据△νOH和加成物生成焓(酸碱作用热)△H的关系,预测了相应酸碱加成物的△H,预测的计算值与实测值符合较好。     

食用油中非食用油的检验

介绍了食用油中含有的桐油、大麻油、蓖麻油、巴豆油、棉籽油及矿物油等非食用油的检验方法,简便易行,对食用油中含有的非食用油成分的检验有一定的参考作用。     

蓖麻油和聚氧乙基蓖麻油的结构和组成的波谱表征

核磁共振波谱法;质谱法;红外光谱法;蓖麻油和聚氧乙基蓖麻油的结构和组成的波谱表征     

Determination of Organophosphorus Pesticides in Soybean Oil, Peanut Oil and Sesame Oil by Low-Temperature Extraction and GC-FPD

A low-temperature clean-up method for residue determination was developed and validated for 14 organophosphorus pesticides in soybean oil, peanut oil and sesame oil by gas chromatography with flame photometric detector (GC-FPD). A different matrix influenced the response and retention time of pesticides. Hence matrix-matched calibration standards were used to counteract the matrix effect. The pesticide responses in blank samples of soybean oil, peanut oil and sesame oil were within the linear range of 0.02–1 mg kg⁻¹ and the correlation coefficients were higher than 0.9989. Average recoveries obtained from different oil samples at three fortified levels were higher than 50% with relative standard deviations (RSDs) of less than 15%. The limit of detections (LODs) of studied pesticides ranged from 2 to 5 μg kg⁻¹. Thirty-nine commercial samples were analyzed, and the results were confirmed by gas chromatography–mass spectrometry (GC–MS) in selective ion monitoring (SIM) mode.     

费谢尔判别法鉴别原油/燃料油

以多环芳烃作为变量,建立了原油、燃料油属性鉴别的费谢尔判别法。分别测定了来自不同国家和地区的26个原油样品和25个燃料油样品中8种多环芳烃的含量,并将它们作为判别变量。借助SPSS 16.0进行费谢尔判别分析,建立费谢尔判别函数。将未知样品的判别变量值代入后,可以快速地得知样品的类别。结果表明,以多环芳烃作为判别变量进行原油、燃料油费谢尔判别快速而准确。     

快速测定植物油胆固醇含量在地沟油筛查中的应用

采用皂化气相色谱氢火焰离子检测器法测试了多个植物油样品,发现胆固醇峰被干扰比较严重,很难得出植物油与地沟油胆固醇含量的界定值。采用SPE进行样品前处理,对SPE处理条件进行优化,得出优化条件为称样量0.25 g ,20 mL 0.6%乙醚-正己烷(V/V)作为淋洗液,20 mL 15%乙醚-正己烷(V/V)作为洗脱液。用SPE气相色谱氢火焰离子检测器法分析了84个植物油样品和13个地沟油样品中胆固醇含量,测定结果表明,植物油胆固醇含量与地沟油胆固醇含量有明显区别,所有植物油胆固醇含量都小于50μg/g,13个地沟油样中11个样胆固醇含量大于50μg/g。因此,采用上述植物油胆固醇测定方法,胆固醇含量超过50μg/g可判定为疑似地沟油,反之不成立。本方法在0~760 mg/L浓度范围内相关系数R2=0.9999,方法检出限为6. 0μg/g,两个浓度水平(17.7和695 mg/L)的相对标准偏差分别为1.6%和1.5%,回收率为103%。     

区分动植物油的气相色谱-质谱分析

在实际办案中,经常需要对附着在不同载体上的油脂斑痕进行检验,嫌疑斑痕为何类何种油脂对案件的侦破有重大意义.各个领域的专家对动植物油的成分进行研究的目的各不相同,食品工业中偏重于动植物油的食用价值,医学中偏重研究油脂对身体的益处或危害,而司法鉴定领域,偏重于对常见油类进行定性分析,从而为侦查破案提供线索.     

Oil and gas production

Colloid and interface science is fundamental to many aspects of oil and gas production processes. This review focuses on recent advances in water-based drilling fluids, reservoir fracturing fluids, polymer gels for modifying reservoir permeability, avoiding problems caused by colloidal asphaltene oil fractions and characterising the wettability of reservoir rocks. There have been major advances in the design and responsiveness of polymer and surfactant fluids, in the understanding and control of shale clayrock swelling and in the relationships between mesoscopic-scale phenomena in porous media and reservoir production performance.     

Neem Oil As Pesticide

Use of synthetic pesticides has resulted into health hazards, ecological imbalance, resistance in pests and environmental pollution.1 Singh, R. 1997. “Studies in formulation of pesticide emulsion”. India: UDCT, University of Mumbai. , Ph.D. Thesis [Google Scholar] Neem oil is natural pesticide and has excellent insecticidal properties. Hence, attempts are being made to develop neem oil emulsions to be used as pesticide. Surfactants like castor‐oil based, nonyl phenol‐based, sodium lauryl sulphate, and calcium alkyl benzene sulphonate were tried to develop stable emulsions. Neem extract based emulsifiable concentrates were prepared by using methanol. Stability of emulsion as a function of type of surfactants, hydrophile‐lipophile balance (HLB) of surfactants and hardness of water was studied. Larvasidal effects of emulsions and emulsifiable concentrates were examined. Laboratory experiments have shown effectiveness of these emulsions and emulsifiable concentrates as pesticide.     

Lipase-Catalyzed Preparation of Diacylglycerol-Enriched Oil from High-Acid Rice Bran Oil in Solvent-Free System

The ability of immobilized lipase from Rhizomucor miehei (Lipozyme RM IM) to catalyze the reaction of high-acid rice bran oil (RBO) and monoglyceride (MG) for diacylglycerol-enriched rice bran oil (RBO-DG) preparation was investigated. The effects of substrate ratio, reaction temperature, time, and enzyme load on the respective content of free fatty acid (FFA) and DG in the final RBO-DG products was investigated. Enzyme screening on the reaction was also investigated. Response surface methodology (RSM) was used to optimize the effects of the reaction temperature (50?C70?°C), the enzyme load (2?C6?%; relative to the weight of total substrates), and the reaction time (4?C8?h) on the respective content of FFA and DG. Validation of the RSM model was verified by the good agreement between the experimental and the predicted values. The optimum preparation conditions were as follows: MG/RBO, 0.25; temperature, 56?°C; enzyme load, 4.77?%; and reaction time, 5.75?h. Under the suggested conditions, the respective content of FFA and DG was 0.28 and 27.98?%, respectively. Repeated reaction tests indicated that Lipozyme RM IM could be used nine times under the optimum conditions with 90?% of its original catalytic activity still retained.