用紫外-可见分光光度计测定油样中沥青质含量

介绍了一种用分光光度法测定油品中的沥青质含量的方法。通过测定样品悬浮液在７５０ｎｍ、８００ｎｍ下的吸光度而获得样品中正庚烷沥青质含量,阐述了方法的测量原理,讨论了取样量范围、沥青地方法的影响。结果表明,该法可应用于各种油品（如原油、重质馏分油、渣油和沥青等）的分析,具有简单、快速的优点,相对标准偏差小于３％。     

Rapid screening of mixed edible oils and gutter oils by matrix-assisted laser desorption/ionization mass spectrometry

Authentication of edible oils is a long-term issue in food safety, and becomes particularly important with the emergence and wide spread of gutter oils in recent years. Due to the very high analytical demand and diversity of gutter oils, a high throughput analytical method and a versatile strategy for authentication of mixed edible oils and gutter oils are highly desirable. In this study, an improved matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) method has been developed for direct analysis of edible oils. This method involved on-target sample loading, automatic data acquisition and simple data processing. MALDI-MS spectra with high quality and high reproducibility have been obtained using this method, and a preliminary spectral database of edible oils has been set up. The authenticity of an edible oil sample can be determined by comparing its MALDI-MS spectrum and principal component analysis (PCA) results with those of its labeled oil in the database. This method is simple and the whole process only takes several minutes for analysis of one oil sample. We demonstrated that the method was sensitive to change in oil compositions and can be used for measuring compositions of mixed oils. The capability of the method for determining mislabeling enables it for rapid screening of gutter oils since fraudulent mislabeling is a common feature of gutter oils.     

Biodegradabilities of some chain oils in groundwater as determined by the respirometric BOD OxiTop method

The respirometric BOD OxiTop method was used to monitor the biodegradation of different chain oils (mineral, rapeseed and tall oils) over 28 days in groundwater, as well as in standard conditions described by OECD 301 F. The aim of the study was to gather more information about the biodegradability of forestry oils in groundwater, as well as about the suitability of the automatic OxiTop method for biodegradation measurements. The BOD OxiTop method proved to be a precise and reliable technique for determining the biodegradations of different oils. Some comparative studies were also made using a traditional IR method in order to clarify the total oil concentrations. The results show that if biodegradation only is to be monitored, the OxiTop method is preferable. This is due to the influence of other reactions aside from biodegradation on total hydrocarbon concentrations when using the IR method.     

Determination of oxidation products in transformer oils using FT-IR spectroscopy

Transformer oils are subject to a lot of control checks in the process of their exploitation, because the presence of oxidized products causes damages in the electrical equipment. In the process of exploitation of transformer oils anti-oxidation additives get exhausted and products of oxidation are formed. This paper describes the development method for study of oxidation transformer oils by Fourier transform infrared (FT-IR) spectroscopy. The aim of this paper is to determine the main products of oxidation of transformer oils and to increase the sensitivity of FT-IR analysis by the extraction method. The method which we suggest to register all oxidized products is of great interest. The problem is the detection limit of routine apparatus. For this reason we have developed an extraction method, which can identify precisely all oxidized products qualitatively and quantitatively in the region 1800-1650 cm⁻¹. Thus a manifold increase of the FT-IR analysis is achieved, combined with increased sensitivity, precision and the possibilities for registering micro-amounts otherwise beyond the routine technique. FT-IR spectroscopy is a powerful method with great practical significance for investigation of carbonyl- and carboxylic degradation products from transformer oils.     

High temperature gas chromatography – atomic emission detection of metalloporphyrins in crude oils

High temperature gas chromatography-atomic emission spectroscopy is used for the detection of vanadyl, nickel, and iron porphyrins in crude oils. The operational variables are investigated with regard to the effects on performance in high temperature GC-AED. Under optimal conditions, the method provides charactersitic metal distributions for oils from different sources. The method is also advantageous in the study of decomposition of petroleum metal species. Several crude oils were analyzed for the content of the distillable metals in comparison with total metals as determined by a direct spectroscopic method.     

Analysis of Peanut Oil Adulterated with Other Edible Oils by Spectrophotometry

Since peanut oil(PO) is more expensive than other seed oils, some PO is adulterated with other cheap seed oils, such as soybean oil, palm olein, cottonseed oil, corn oil and rapeseed oil. The conventional method for determining whether PO was adulterated is to detect the freezing point of oils. The proposed method for the determination of adulterants in PO was based on monitoring the change of absorbance when the sample was refrigerated. A special spectrophotometer was developed. A total of 10 kinds of POs from different suppliers were chosen and adulterated with other seed oils at the volume fraction levels ranging from 5% to 30%. A total of 150 samples were analyzed by the proposed method and the results were satisfactory.     

原油烃指纹GC法在三元复合驱油井分层产能测试中的应用

通过三元复合液与水驱原油作用实验认为,三元复合液对原油烃指纹影响小;通过分层原油配比实验及测试与MFE法分层测试结果对比认为,两种测试方法具有很好的一致性,原油烃指纹色谱测试法适用于三元复合驱油井,为三元复合驱油井分层产能测试及驱油效果监测提供了有效的方法。     

常压火焰离子化质谱技术对食用植物油快速分析的初探

建立了常压火焰离子化质谱(Ambient flame ionization mass spectrometry,AFI-MS)快速分析食用植物油(橄榄油、芝麻油、花生油和葵花籽油)的方法。AFI-MS检出食用植物油(橄榄油、芝麻油、花生油和葵花籽油)中的26种甘油三酯和11种甘油二脂。AFI-MS分析显示,不同的食用植物油(橄榄油、芝麻油、花生油和葵花籽油)得到的质谱图轮廓信息不同。通过对不同食用植物油的甘油三酯相对峰强度进行分析,可初步归纳出食用植物油的类型。AFI-MS分析食用植物油的操作简单,普通的打火机就可以作为离子源用于食用植物油的分析。这种便捷的离子化技术可以用于食用植物油的快速分析。     

Study and isolation of vanadylporphyrins from the petroleum oils of the Buzachi peninsula

Summary 1. The vanadylporphyrin complexes of the petroleum oils of the Buzachi peninsula have been studied by the ESR method and spectrophotometrically. The results of the investigation show that the ESR method is the most convenient for determining small amounts of vanadylporphyrins in petroleum oils and extracts.2. The selectivity of various solvents in the extraction of vanadylporphyrin complexes from petroleum oils, as determined by the ESR method, is discussed.Institute of the Chemistry of Petroleum and Natural Salts, Academy of Sciences of the Kazakh SSR, Gur'ev. Translated from Khimiya Prirodnykh Soedinenii, No. 3, pp. 389–392, May–June, 1978.     

A capillary electrophoresis-tandem mass spectrometry methodology for the determination of non-protein amino acids in vegetable oils as novel markers for the detection of adulterations in olive oils

A new analytical methodology based on capillary electrophoresis-mass spectrometry (CE-MS(2)) is presented in this work, enabling the identification and determination of six non-protein amino acids (ornithine, β-alanine, GABA, alloisoleucine, citrulline and pyroglutamic acid) in vegetable oils. This methodology is based on a previous derivatization with butanol and subsequent separation using acidic conditions followed by on-line coupling to an ion trap analyzer for MS(2) detection established through an electrospray-coaxial sheath flow interface. The electrophoretic and interface parameters were optimized obtaining the separation of all compounds in less than 15 min and with resolutions higher than 5. The proposed method was validated by assessing its accuracy, precision (RSD<7% for corrected peak areas), LODs and LOQs (between 0.04-0.19 ng/g and 0.06-0.31 ng/g, respectively) and linearity range (R(2)>0.99), and it was used in order to identify the selected non-protein amino acids in soybean oils, sunflower oils, corn oils and extra virgin olive oils. MS(2) experiments performed the fingerprint fragmentation of these compounds allowing to corroborate ornithine and alloisoleucine in seed oils but not in olive oils. The method was applied to identify and quantify olive oil adulterations with soybean oil detecting in a single run the amino acids in mixtures up to 2% (w/w). The results showed a high potential in using these compounds as novel markers for the detection of adulterations of extra virgin olive oils with seed oils. Thus, the developed method could be considered a simple, rapid and reliable method for the quality evaluation of extra virgin olive oil permitting its authentication.     

Salvia officinalis L. essential oils: effect of hydrodistillation time on the chemical composition, antioxidant and antimicrobial activities

Salvia officinalis L. oils were isolated from the plant's commercial dried aerial parts, by hydrodistillation, with different distillation times. The essential oils were analysed by gas chromatography and gas chromatography-mass spectrometry. The antioxidant ability was measured using a free radical scavenging activity assay using 2,2-diphenyl-1-picrylhydrazyl (DPPH), a thiobarbituric acid reactive substances (TBARS) assay, a deoxyribose assay for the scavenging of hydroxyl radical, an assay for site-specific actions and a 5-lipoxygenase assay. Antibacterial activity was determined by the agar diffusion method. 1,8-Cineole, α-pinene and camphor were the dominant components of all the essential oils. The different hydrodistillation times did not affect the oil yield nor the relative amount of the oil components. The time of hydrodistillation influenced the antioxidant activity. With the DPPH method, the oils isolated for 2 and 3 h were stronger free radical scavengers, while with the TBARS method, the highest antioxidant values were obtained in the oils isolated for 30 min, 2 and 3 h. Hydroxyl radical scavenging and lipoxygenase activity assays showed the best results with oils isolated for 1 and 3 h. With the deoxyribose method, sage oils at concentrations <1000 mg L(-1) showed better activity than mannitol. The essential oil of S. officinalis showed very weak antimicrobial activity.     

SPME/GC-MS鉴别地沟油新方法

采用固相微萃取(SPME)气相色谱-质谱联用(GC-MS)技术,研究了油脂内源及外源物质的微量化学成分。结果发现:纯正花生油和大豆油不含反式脂肪酸,地沟油含有反式脂肪酸trans-C18∶1、trans-C18∶2;纯正花生油和大豆油中含有正己醛、正壬醛和正癸醛等杂质,而地沟油中除了这几种醛类外还含有乙酸、3-丁烯腈、2,5-二甲基吡嗪等特征杂质成分。通过测定内源性物质和外源性物质的存在,两种检测结果互相印证,综合判断,最终可确定是否为地沟油,据此首次建立了SPME/GC-MS鉴别地沟油的新方法。该方法不但可用于地沟油的鉴别,还可用于掺假食用油的检测。     

Entwicklung und Anwendung einer auf IR-, NMR-Spektroskopie und Elementaranalyse beruhenden Strukturgruppenanalyse für höhersiedende Kohlenwasserstoffgemische und Mineralölanteile

From an input of 8 measured numbers it provides 35 statistical informations on structure. The reliability of the method is demonstrated from a series of oil mixtures. The results for two oils are compared with those from a similar method. The application is proved from results of a large number of technical oils and GPC fractions from crude oils.     

气相色谱–质谱法测定食用植物油中23种农药残留

建立了测定食用植物油中23种农药残留的气相色谱–质谱联用方法。采用固相萃取,以乙腈超声提取,经过PSA,C_(18)柱进行净化,用气相色谱–质谱法测定,外标法定量。23种农药在0.01~1.0 mg/L范围内与色谱峰面积线性关系良好,相关系数为0.997 3~0.999 7,方法检出限为5~15μg/kg。测定结果的相对标准偏差为2.25%~9.40%(n=6),加标回收率为78.4%~127.3%,可以满足食用植物油中多种农药残留的同时分析。采用该方法对国内市场常见的食用植物油进行检测分析,所检测的农药残留均在国家标准的限量范围内。     

Study of the phenolic composition of spanish and italian monocultivar extra virgin olive oils: Distribution of lignans, secoiridoidic, simple phenols and flavonoids

The aim of the present study was to compare the phenolic content in selected monocultivar extra virgin olive oils. Analyses were carried out by HPLC/DAD/MS on Picual, Picuda, Arbequina and Hojiblanca oils from Spain and Seggianese and Taggiasca oils from Italy. Oils from cultivar Picual showed similar characteristics to those of Seggianese oils, with total amounts of secoiridoids of 498.7 and 619.2 mg/L, respectively. The phenolic composition of Arbequina oils is close to that of the Taggiasca variety with lignans among the main compounds. The determination of free and linked OH-Tyr, by way of an acid hydrolysis, represents a rapid and suitable method, especially when standards are not available, to determine antioxidant potentialities in terms of MPC, particularly for fresh extra virgin olive oils rich in secoiridoidic derivatives.     

气质联用结合保留指数对比在五种木兰科芳香精油成分鉴定中的应用

采用气相色谱-质谱联用技术结合Kovats保留指数（KI）比较法，对南岭自然保护区内野生的毛桃木莲、乳源木莲、乐昌含笑、金叶含笑和深山含笑等5种木兰科芳香植物精油进行了化学成分对比鉴定。结果表明，这种方法与单纯质潜匹配度的方法相比，大大提高了组分化学物质鉴定的准确性。除深山含笑外，另外4种木兰科芳香精油所含的大部分成分均为倍半萜类，，毛桃木莲和乳源木莲精油在基本组分构成上具有高度一致性，且在主要成分上具有相似性，这表明它们可能具有非常近的植物亲缘关系。乐昌含笑和金叶含笑精油均以倍半萜类为主体成分，深山含笑精油则以单萜烯类为主体成分，这3种含笑属芳香精油在组分构成上没有明显的一致性。     

A novel infrared spectrophotometric method for the rapid determination of petroleum hydrocarbons, and animal and vegetable oils in water

To determine the concentrations of total oils,petroleum hydrocarbons,and animal and vegetable oils in water,the conventional analytical methods involve two scans as well as a step of magnesium silicate adsorption to remove the animal and vegetable oils in water samples.In this study,a novel analytical method was developed to determine the above oils in wastewater samples through just one scan—the concentration of animal and vegetable oils,and that of total oils were determined by measuring the absorbance of the >C=O bond in the peak area between 1750 cm and 1735 cm^-1,and of the C-H bond at 2930 cm^-1,2960 cm,and 3030 cm^-1,respectively.The concentration of petroleum hydrocarbons was then calculated by subtracting the concentration of animal and vegetable oils from that of total oils.Compared with the well-known analytical method GB/T 16488-1996,the novel approach displayed similar accuracy in the quantitative determination of oils in wastewater samples,but significantly reduced material cost and operation time.     

Concentration dependent red shift: qualitative and quantitative investigation of motor oils by synchronous fluorescence scan

Synchronous fluorescence scan (SFS) has been described as a successful technique to characterize Motor oils like diesel, petrol, kerosene, 2T oil and Mobil. The concentration dependent investigation of Motor oils shows a red shift in lambda(SFS)(max). Using red shift of lambda(SFS)(max), a method has been developed to quantify Motor oil in the concentration range 5-100% v/v. The concentration dependent overall rate of energy transfer of Motor oil gives a unique behavioral change according to the oil type and SFS is a simpler spectroscopic method to qualitatively differentiate between heavy and light oil. The molecular interaction of polycyclic aromatic compounds (PACs) in fluorophoric mixtures like resonance energy transfer and self-quenching via solvent collision has been clearly explained by SFS method. Effect of solvent and external quencher molecule on Motor oils has also been studied. Nitrobenzene is found to be a selective quencher for PACs of Motor oils.     

Evaluation and Optimization of the Oxidation efficiency of a UV-Persulphate-Oxidation Toc-Analyzer for the Determination of Oil Contamination from Forestry in Ground Water

Different chain oils (tall, rape seed and mineral oils) have been used as model compounds to evaluate and optimize the applicability of UV-persulphate TOC-analyzer for quantitative determination of forestry oils and to follow the progress of their biodegradability. It was shown, that K 2 S 2 O 8 -UV-oxidation method is not sufficient to oxidize chain oils completely. There were differences in oxidation efficiency between different oils, changing from about 46% measured for tall oil to about 25% observed for rape seed chain oil. The addition of Triton X-100 surfactant up to 2% (w/w) was observed to increase the oxidation efficiency, e.g. to 75% for tall oil. The observations can be explained by assuming that in the presence of surfactant the emulsions are more homogeneous and stable. Optimization using two-level full factorial design (temperature of the oxidation chamber and the amount of persulphate) was studied. The results show that the UV-persulphate-oxidation TOC-analyzer is not suitable method to monitor biodegradability of chain oils.     

GC-MS与交互移动窗口因子分析法(AMWFA)用于3种陈皮挥发油成分的比较分析

将GC-MS法与新近提出的用于二维数据比较和解析的交互移动窗口因子分析法(AMWFA)结合, 对3种不同原植物来源的陈皮挥发油成分的共性和差异性进行分析, 并对重叠峰进行解析, 总共分辨出138个峰, 定性出78个峰, 其中共有组分44个.