Determination of pesticide residues in olives and olive oil by matrix solid-phase dispersion followed by gas chromatography/mass spectrometry and liquid chromatography/tandem mass spectrometry

A novel analytical approach has been developed and evaluated for the quantitative analysis of a selected group of widely used pesticides (dimethoate, simazine, atrazine, diuron, terbuthylazine, methyl-parathion, methyl-pirimiphos, endosulfan I, endosulfan II, endosulfan sulphate, cypermethrin and deltamethrin), which can be found at trace levels in olive oil and olives. The proposed methodology is based on matrix solid-phase dispersion (MSPD), (with a preliminary liquid-liquid extraction in olive oil samples) using aminopropyl as sorbent material with a clean-up performed in the elution step with Florisil, followed by mass spectrometric identification and quantitation of the selected pesticides using both gas chromatography-mass spectrometry (GC-MS) in selected ion monitoring (SIM) mode and liquid chromatography tandem mass spectrometry (LC-MS-MS) in positive ionization mode. The recoveries obtained (with mean values between 85 and 115% (obtained at different fortification levels) with RSD values below 10% in most cases, confirm the usefulness of the proposed methodology for the analyses of these kind of complex samples with a high fat content. Moreover, the obtained detection limits, which were below 5 microg kg(-1) by LC-MS analyses and ranged from 10 to 60 microg kg(-1) by GC-MS meet the requirements established by the olive oil pesticide regulatory programs. The method was satisfactorily applied to different olives and olive oil samples.     

Chemical Composition of the Essential Oil of <Emphasis Type="Italic">Salvia macilenta</Emphasis> from Iran

The hydrodistilled essential oil composition from the aerial parts of Salvia macilenta (Lamiaceae) from Iran was analyzed by GC and GC-MS. The oil analysis confirmed the characterization of thirty-one compounds, accounting for 99.4% of the total oil. Analysis of the oil showed that the oil of S. macilenta was rich in monoterpene hydrocarbons with a-pinene (60%) as the main component followed by γ-elemene (6.1%), thymol (5.2%), elemol (4.7%), and β-caryophyllene (4.1%).__________Published in Khimiya Prirodnykh Soedinenii, No. 2, pp. 136–137, March–April, 2005.     

硅胶与高岭土的润湿性及荧光和驱油研究

利用Washburn方程测量固体粉末的润湿性,研究了十二烷基苯磺酸钠(SDBS)水溶液在硅胶及高岭土两种固体粉末表面上的接触角,用荧光猝灭法测定了SDBS在水溶液里的胶束平均聚集数。并由此探讨了十二烷基苯磺酸钠水溶液在固体粉末表面的润湿性,表面活性剂的临界胶束浓度(CMC)与表面含油粉末脱油率的关系。     

Die geruchsintensivsten Inhaltsstoffe des ostindischen Sandelholzöles

The most odour intensive constituents of east indian sandal wood oil are -santalol, -santalal and -santalene. This has been proved by a thorough GLC-investigation in combination with the sniffing technique of seven fractions of this highly priced essential oil, which have been obtained by TLC on silica-cellulose plates with simultaneous organoleptic evaluation. Using the headspace analysis these results could be confirmed and further the distribution of the main odour components was obtained in headspace at 37° and 80°.

Herrn Prof. DDr. h. c.K. Kratzl in dankbarer Verehrung mit den besten Wünschen zum 70. Geburtstag gewidmet.     

磁化后掺水乳化重油分散度的实验研究

乳化重油的分散相（水）微粒大小对重油掺水乳化燃烧技术的应用效果有很大影响,本人在过去实验的基础上,用光学反射显微镜法对磁场作用下掺水乳化重油中分散相（水）的分散度进行了测定,研究了乳化重油的分散度与磁场强度、温度以及流速之间的关系,实验结果表明：磁化后有利于乳化重油的微细化,且效果比较显著;温度的升高有利于分散相（水）的微细化,兼顾能耗和燃油的发泡、沸腾现象,以及磁化后温度的升高对分散度的影响减少,有一个合理的温度范围;磁化后分散度与流速的关系呈峰值关系,本实验中流速较佳值为8m/s;磁场强度的增大也有利于微细化,磁场强度太高或太低均不会取得太好的处理效果,在1000GS－1400GS范围内为宜。     

磁场作用下乳化重油稳定性的实验研究

燃油磁化燃烧技术是一种新的燃烧技术 ,目前以日本发展较快[1,2 ] ,其节能效果也已为实践所证实[3～ 5] 。我们知道 ,掺水乳化重油稳定性好 ,燃烧状况就稳定 ;稳定性差 ,油水在进入炉膛燃烧前就已分层 ,不但起不到“微爆”效果 ,而且严重时导致熄火。作者曾对未磁化乳化重油的粘度、稳定性和分散度进行了实验研究[6～ 8] ,丘纪华等学者[9～ 11] 对磁化技术在石油、化工、燃料等方面的作用机理及应用进行了一定的研究 ,但是重油掺水乳化后再经磁化处理后其稳定性发生怎样的变化 ,尚未见实验报道。因此 ,为了更好地发挥这一技术的节油和环保效…     

轻质油料电导率仪检定方法研究

叙述轻质油料电导率仪的检定原理及检定方法。采用高阻结合标准物质的方法解决了轻质油料电导率仪无法检定的问题。     

残留Na对镍催化剂加氢性能的影响

采用共沉淀的方法制备了以镍为活性组分、镁为助剂、 SiO_2为载体的Ni-Mg/SiO_2催化剂,以大豆油加氢为探针反应研究催化剂中残留Na的含量对加氢活性的影响.分别用ICP-AES、 XRD、 H_2-TPR、 TG-DSC、 SEM、 BET等手段对不同催化剂进行了表征.结果表明:催化剂中残留Na对加氢活性有很大影响, Na含量为6.86%时,催化剂基本没有活性.随Na含量的降低,催化剂活性逐渐升高.这主要是由于Na对Ni的分散、颗粒尺寸和与载体相互作用有较大的影响有关.     

尿素改性β-分子筛催化苯与煤制油烷基化制重烷基苯

对β-分子筛(n(Si)：n(Al)=15：1)分别进行酸洗、碱洗改性,制备出孔结构、酸性等性质不同的分子筛催化剂。 通过扫描电子显微镜(SEM)、X射线衍射(XRD)、N₂吸附-脱附、NH₃-TPD和Py-FTIR等表征手段对分子筛催化剂的结构、性能及其在苯的烷基化反应中的应用进行了研究。 结果表明,盐酸浸洗对β-分子筛的孔径、比表面积及孔容均有扩大作用,但在酸性上有所减弱;NaOH溶液浸洗造成了分子筛骨架的崩塌,对其酸性与孔结构均造成了破坏;尿素改性不仅改善了分子筛的孔结构性质,而且对分子筛酸性影响较小,是一种温和、有效的改性方式。 尿素改性β-分子筛催化剂催化苯与煤基冷阱油的烷基化反应活性最好,烯烃转化率达91.2%,且重烷基苯2位异构体(2-HAB)和3位异构体(3-HAB)在产物中含量最高,选择性分别为50.1%和33.5%,占整个烷基化产物的84%。