同时测定食用植物油中抗氧剂叔丁基对羟基茴香醚和2，6－二叔丁基对甲酚的方法

 报道了用高效液用色谱法同时测定食用植物油中的抗氧剂叔丁基对羟基茴香醚（ＢＨＡ）和２，６－二叔丁基对甲酚（ＢＨＴ）的实验方法。采用ＺｏｒｂａｘＯＤＳＣ_（１８）色谱住，甲醇：水（９０：１０，Ｖ／Ｖ）作流动相，检测波长为２４５ｎｍ，流速为１ｍＬ／ｍｉｎ。检测下限分别为１５ｎｇ（ＢＨＡ），９０ｎｇ（ＢＨＴ），回收率分别是９６．８％±９．８％（ＢＨＡ），９９．０％±３．２％（ＢＨＴ）。方法快速、准确，灵敏度高。     

铂—钯共显色衍生络合物的高效液相色谱研究

研究了Ｐｄ（Ⅱ）和４，４＇－二（二乙氨基）苯硫酮（ＢＤＰＴＫ）共显色所生成的Ｐｔ（Ⅱ）络合物，于Ｎｕｃｌｅｏｓｉｌ Ｃ８柱上，用含３×１０＾－３ｍｏｌ／Ｌ ＣＳＡ和０．０２ｍｏｌ／Ｌ ＨＡｃ－ＮａＡｃ（ｐＨ３．５）的乙腈－丙酮－水（７２：５：２３，Ｖ／Ｖ）作流动相（１．０ｍｌ／ｍｉｎ）分离并检测。Ｐｔ的校正曲线的线性范围为０．２～３．０μｇ／ｍｌ，Ｐｔ检测限为０．７ｎｇ。此方法已应用于抗癌药物顺铂     

锆—7—碘—8—羟基喹啉—5—磺酸—EDTA—表面活性剂体系的荧光光度法研究

在ｐＨ６．２的ＨＡｃ－ＮａＡｃ缓冲溶液中，在溴化十六烷基三甲基胺（ＣＴＭＡＢ）存在下，Ｚｒ（Ⅳ）与７－碘－８－羟基喹啉－５－磺酸（Ｈ２ＱＳＩ）及ＥＤＴＡ形成了四元荧光配合物，其组成为：Ｚｒ：Ｈ２ＱＳＩ：ＥＤＴＡ：ＣＴＭＡＢ＝１：１：１：３。据此建立了锆的选择性好，灵敏度高的荧光测定方法，方法检测限为１．２ｎｇ／ｍＬ。锆的线性范围为１．６ｎｇ～１．０μｇ／ｍＬ。用于铜合金中微量锆的测定，结果令人满意     

锆－7－碘－8－羟基喹啉－5－磺酸－EDTA－表面活性剂体系的荧光光度法研究

在ｐＨ６．２的ＨＡｃ－ＮａＡｃ缓冲溶液中，有溴化十六烷基三甲基铵（ＣＴＭＡ８）存在下，Ｚｒ（Ⅳ）与７－碘－８－羟基喹啉－５－磺酸（Ｈ＿２ＱＳＩ）及ＥＤＴＡ形成了四元荧光配合物。其组成为：Ｚｒ：Ｈ＿ＱＳＩ：ＥＤＴＡ：ＣＴＭＡＢ＝１：１：１：３。据此建立了错的选择性好、灵敏度高的荧光测定方法。方法检测限为１．２ｎｇ／ｍＬ。锆的线性范围为１．６ｎｇ～１．０μｇ／ｍＬ。用于铜合金中微量锆的测定，结果令人满意。     

HPLC/ECD测定人血小板中5-羟色胺浓度

用ＨＰＬＣ／ＥＣＤ法测定血小板５－ＨＴ,运用 ＷａｔｅｒｓμＢｏｎｄａｐａｋ Ｃ柱,３,４二羟基苄胺（ＤＨ－ＢＡ）作内标,以 ０.０７ ｍｏｌ／Ｌ乙酸钠缓冲液＋乙腈为流动相（２０＋１）,每１Ｌ缓冲液含 ０．０５ ｍｏｌ／Ｌ柠檬酸、２．５ ｍｍｏｌ／Ｌ庚烷磺酸钠、０．１ｍｍｏｌ／Ｌ Ｎａ_２ＥＤＴＡ,流速０．８ ｍＬ／ｍｉｎ。ＤＨＢＡ和 ５－ＨＴ的保留时间分别为５．４和１１．５ ｍｉｎ,线性范围为０．０２５～１ｍｇ／Ｌ（ｒ＝ ０．９９９７）。５－ＨＴ日内 ＲＳＤ低于１．８７％,日间ＲＳＤ低于８．５４％,方法回收率为１００．４％±２．３％。提示本方法快速简便,灵敏准确,适用于临床基础研究。     

4－（6－甲基－2－苯并噻唑偶氮）间苯三酚反相高效液相色谱分离测定钒钴镍铬

作者以新研制的４－（６－甲基－２－苯并噻唑偶氨）间苯三酚为柱前衍生试剂，用含１０ｍｍｏｌ／Ｌ的ｐＨ６．８０的ＨＡｃ－ＮａＡｃ缓冲溶液，１０ｍｍｏｌ／ＬＴＢＡ·Ｂｒ和１×１０￣（－４）ｍｏｌ／ＬＥＤＴＡ的甲醇－水溶液（７８：２２，Ｖ／Ｖ）作流动相，在Ｃ＿（１８）柱上，１１ｍｉｎ内反相ＨＰＬＣ分离测定了Ｃｒ（Ⅵ），Ｖ（Ⅴ）Ｃｏ（Ⅱ），Ｎｉ（Ⅲ）。当Ｓ／Ｎ＝３时，其检出限分别是Ｖ（Ⅴ）５．４５ｎｇ，Ｃｏ（Ⅱ）１．０９ｎｇ，Ｎｉ（Ⅱ）１．５０ｎｇ，Ｃｒ（Ⅵ）１．７０ｎｇ。     

高效液相色谱法快速测定食品中抗氧化剂BHA,BHT

采用甲醇浸提食品样品中抗氧化剂ＢＨＡ（叔丁基羟基茴香醚）和ＢＨＴ（二叔丁基羟基甲苯），然后用高效液相色谱法测定提取液中的ＢＨＡ和ＢＨＴ。该法简单快速，准确性好，ＢＨＡ和ＢＨＴ的最小检出量分别为５ｎｇ和１０ｎｇ。     

高碘酸盐氧化罗丹明B催化光度法测定钌

在０．７２ｍｏｌ／Ｌ磷酸和９０℃水浴条件下,钌催化高碘酸盐氧化罗丹明Ｂ（ＲＢ）,据此建立了高灵敏催化光度测定钌的方法。方法的检出限为８．０×１０＾－１２ｇ／ｍＬ,测定范围为０．２～１５ｎｇ／２５ｍＬ,对５、１０、１５ｎｇ／２５ｍＬＲｕ（Ⅲ）测定的相对标准偏差分别为８．６７％,５．９４％和１．８５％。本反应对Ｒｕ（Ⅲ）、ＲＢ、ＫＩＯ４和Ｈ３ＰＯ４均为一级反应,表观活化能为３６．０５ｋＪ／ｍｏｌ。１３     

氢化物发生—缝管原子捕集—原子吸收法测定钢铁和地质试样中的砷

介绍简易的氢化物发生原子吸收测砷的方法，喷雾器负压将ＫＢＨ５吸入反应器，并将生成的ＡｓＨ３吸入乙炔－空气焰原子化。石英缝管使灵敏度提高３．５倍，方法的检测限为１．８ｎｇ／ｍＬ（５ｍＬ试样）。２０ｎｇ／ｍＬ Ａｓ（Ⅲ）标准液１０次测定的ＲＳＤ为３．８％。本法成功地应用于钢铁和地质标样中微量砷的测定。     

反相离子对色谱分析水稻愈伤组织中的内源生长素

本文用反相离子对色谱技术定量分析了水稻愈伤组织中的内源生长素５０Ｈ－１ＡＡ和１ＡＡ，样品用８０％丙酮－ＢＨＴ－抗坏血酸抽提，经ＤＥＡＥ纤维素柱和ＸＡＤ－７吸附树脂柱净化和富集，在Ｌｉｃｈｒｏｓｏｒｂ ＲＰＣ１８柱上分离，荧光检测。最低检出限：１ＡＡ为８０ｐｇ，５０Ｈ－ＩＡＡ为０．３ｎｇ。回收率为８５．５％～７３．３％，相对标准偏差为２．２％。文中还对ｐＨ值和离子对试剂对保留值的影响，进行了讨论，对     

气相-质谱选择离子法测定化妆品中抗氧化剂丁基羟基茴香醚、二丁基羟基甲苯

 采用气相 质谱 (选择离子方式 )测定化妆品中抗氧化剂丁基羟基茴香醚 (BHA)和二丁基羟基甲苯(BHT) ,样品用甲醇振荡萃取 ,以SupelcoWAXTM 10 (30m× 0 2 5mmi.d .× 0 2 5 μm)为分析柱。该方法对样品中BHA和BHT的检测限分别为 2 5 μg/g和 0 5 μg/g。方法简便、快速、灵敏 ,可用于多种化妆品的检验。     

Sodium Butylated Hydroxytoluene (NaBHT) as a New and Efficient Hydride Source for Pd-Catalysed Reduction Reactions

NaBHT (sodium butylated hydroxytoluene), a hindered and soluble base for the efficient arylation of various base-sensitive amines and (hetero)aryl halides has been found to have an unanticipated role as a hydride donor to reduce (hetero)aryl halides and allylic acetates. Mechanistic studies have uncovered that NaBHT, but not BHT, can deliver multiple hydrides through oxidation of the benzylic methyl group in NaBHT to the aldehyde. Further, performing the reduction with NaBHT-d₂₀ has revealed that the redox-active benzylic position is not the only hydride donor site from NaBHT with one hydride in three coming, presumably, from the tert-butyl groups. The reduction works well under mild conditions and, incredibly, only consumes 20 percent of the NaBHT in the process; the remaining 80 percent can be readily recovered in pure form and reused. This, combined with the low cost of the material in ton-scale quantity, makes it practical and attractive for wider use in industry at scale.     

基于Au NPs@NU-901电化学传感器检测饼干中丁基羟基茴香醚的研究

基于金属有机骨架的拓扑三维结构的高比表面积以及金纳米颗粒(Au NPS)的优异电催化活性,金纳米颗粒与金属有机框架的复合材料在电化学传感领域拥有应用潜力。该文成功合成了Au NPs@NU-901复合材料,并采用透射电镜、X射线衍射、红外光谱以及X射线光电子能谱对其进行表征。采用线性扫描伏安法和差分脉冲伏安法研究了复合材料对丁基羟基茴香醚(BHA)电化学氧化反应的催化能力。结果表明,Au NPs@NU-901对BHA的电化学氧化具有较好的催化能力。基于Au NPs@NU-901制备电化学传感器用于BHA的定量检测,BHA的氧化峰电流与其浓度在0.10~50 μmol/L范围内呈现良好线性关系,相关系数(r2)为0.994 8,检出限(S/N=3)为0.049 μmol/L,相对标准偏差(RSD)为3.6%。将该传感器应用于饼干样品中BHA的检测,加标回收率为95.6%~104%,样品检测结果与高效液相色谱法的测定结果吻合。方法的选择性好、灵敏准确,适合于饼干中BHA的检测。     

New Multifunctional Agents Based on Conjugates of 4-Amino-2,3-polymethylenequinoline and Butylated Hydroxytoluene for Alzheimer’s Disease Treatment

New hybrids of 4-amino-2,3-polymethylenequinoline with different sizes of the aliphatic ring linked to butylated hydroxytoluene (BHT) by enaminoalkyl (7) or aminoalkyl (8) spacers were synthesized as potential multifunctional agents for Alzheimer’s disease (AD) treatment. All compounds were potent inhibitors of acetylcholinesterase (AChE) and butyrylcholinesterase (BChE) with selectivity toward BChE. Lead compound 8c, 2,6-di-tert-butyl-4-{[2-(7,8,9,10- tetrahydro-6H-cyclohepta[b]quinolin-11-ylamino)-ethylimino]-methyl}-phenol exhibited an IC₅₀(AChE) = 1.90 ± 0.16 µM, IC₅₀(BChE) = 0.084 ± 0.008 µM, and 13.6 ± 1.2% propidium displacement at 20 μM. Compounds possessed low activity against carboxylesterase, indicating likely absence of clinically unwanted drug-drug interactions. Kinetics were consistent with mixed-type reversible inhibition of both cholinesterases. Docking indicated binding to catalytic and peripheral AChE sites; peripheral site binding along with propidium displacement suggest the potential of the hybrids to block AChE-induced β-amyloid aggregation, a disease-modifying effect. Compounds demonstrated high antioxidant activity in ABTS and FRAP assays as well as inhibition of luminol chemiluminescence and lipid peroxidation in mouse brain homogenates. Conjugates 8 with amine-containing spacers were better antioxidants than those with enamine spacers 7. Computational ADMET profiles for all compounds predicted good blood-brain barrier distribution (permeability), good intestinal absorption, and medium cardiac toxicity risk. Overall, based on their favorable pharmacological and ADMET profiles, conjugates 8 appear promising as candidates for AD therapeutics.     

Determination of Butylated Hydroxyanisole by Briggs‐Rauscher Oscillating Reaction Catalyzed by a Macrocyclic Nickel (II) Complex

A novel analytical approach for quantitative measurement of butylated hydroxyanisole (BHA) is dis‐ cussed in this paper. Such a method depends on the inhibitory effect of BHA on a Briggs‐Rauscher (B‐R) oscillating reaction. Unlike the classical B‐R system which involves Mn²⁺ as the catalyst, such a B‐R sys‐ tem is catalyzed by a macrocyclic nickel (II) complex [NiL](ClO₄)₂, where L in the complex is an unsatu‐ rated ligand 5,7,7,12,14,14‐hexemethyl‐1,4,8,11‐tetraazacyclotetradeca‐4,11‐diene. By perturbation of BHA on the system, the oscillation was inhibited in the presence trace amounts of BHA and the inhibition time was found to be proportional to the concentration of BHA over the range 1.00×10^?7–1.20×10^?4 mol/L. Two calibration curves were obtained: the first linear regression is over the range of 1.00×10^?7–2.00×10^?6 mol/L, and the second linear regression is over the range between 2.00×10^?6 and 1.20×10^?4 mol/L, with a lowest limit of detection of 4.00×10^?8 mol/L. UV spectra measurements were employed to clarify the possible perturbation mechanism caused by BHA on the B‐R oscillating reaction.     

四（五氟化苯基）卟啉氯化铁选择催化氧化超临界丙烷的反应机理

 以BHT为自由基捕捉剂，研究了四（五氟化苯基）卟啉氯化铁（Ⅲ）将超临界丙烷高选择性催化氧化为丙醇的反应机理．通过GC－MS分析发现，反应产物中有PBHT，故可认为在超临界丙烷氧化反应过程中有丙基自由基存在，初步推断反应涉及自由基机理．同时发现高浓度BHT抑制反应，低浓度BHT促进反应的现象，而以戊烷为底物时没有促进作用．这是由于BHT的位阻效应所致．并对BHT存在时超临界丙烷氧化反应机理进行了初步的推断．     

合成2,6-叔丁基对甲酚的气相色谱分析

本文介绍了对甲酚与混合C4以杂多酸为催化剂合成2.6 二叔丁基对甲酚(BHT)的气相色谱分析。此方法使用Φ3×3m不锈钢填充柱,内装涂有10%SE 30的白色硅烷化101担体,FID检测器,已知物对照法及色质联用定性。该方法测定了样品中12种化合物,以扣除溶剂的面积归一法定量。     

Determination of BHT in the presence of surfactants using a cellulose acetate coated electrode and square wave voltammetry

A direct voltammetric method for the rapid determination of butylated hydroxytoluene has been developed. The procedure utilizes a hydrolyzed cellulose acetate film in intimate contact with a glassy carbon electrode and square wave voltammetry. The coated electrode prevents passivation due to adsorption of polymeric oxidation products by way of a size exclusion principle. BHT solutions containing lipid-like surfactants can be analyzed without the need for frequent resurfacing of the electrode.     

吸热型碳氢燃料裂解引发剂筛选及引发机理分析

筛选可溶性添加剂替代多相催化剂, 达到促进吸热型碳氢燃料裂解、提高燃料热沉以及燃烧性能的目的. 采用考察裂解气相产物气体流量的方法进行实验. 测试了10种添加剂在500～650 ℃范围内对正庚烷裂解效果的影响. 研究发现, 三乙胺、2,6-二叔丁基对甲酚(BHT)可促进正庚烷裂解, 其它添加剂均无显著效果. 在550 ℃时, 当三乙胺质量分数达到6%时, 实验总气体收率比计算总气体收率增加80%以上. 机理研究表明, 三乙胺的引发剂基团来源于C—N键的断裂. BHT的结构、性状与前者显著不同, 在550 ℃时, 当BHT质量分数为3.4%时体系的气体收率较之纯正庚烷裂解气体收率增加80%以上, BHT的引发基团主要是连接于叔丁基上的甲基发生脱离的结果     

Butylated hydroxytoluene analogs: synthesis and evaluation of their multipotent antioxidant activities

A computer-aided predictions of antioxidant activities were performed with the Prediction Activity Spectra of Substances (PASS) program. Antioxidant activity of compounds 1, 3, 4 and 5 were studied using 1,1-diphenyl-2-picrylhydrazyl (DPPH) and lipid peroxidation assays to verify the predictions obtained by the PASS program. Compounds 3 and 5 showed more inhibition of DPPH stable free radical at 10?? M than the well-known standard antioxidant, butylated hydroxytoluene (BHT). Compound 5 exhibited promising in vitro inhibition of Fe2?-induced lipid peroxidation of the essential egg yolk as a lipid-rich medium (83.99%, IC?? 16.07 ± 3.51 μM/mL) compared to α-tocopherol (α-TOH, 84.6%, IC?? 5.6 ± 1.09 μM/mL). The parameters for drug-likeness of these BHT analogues were also evaluated according to the Lipinski’s “rule-of-five” (RO5). All the BHT analogues were found to violate one of the Lipinski’s parameters (LogP > 5), even though they have been found to be soluble in protic solvents. The predictive polar surface area (PSA) and absorption percent (% ABS) data allow us to conclude that they could have a good capacity for penetrating cell membranes. Therefore, one can propose these new multipotent antioxidants (MPAOs) as potential antioxidants for tackling oxidative stress and lipid peroxidation processes.