Automated on-line gel permeation chromatography-gas chromatography for the determination of organophosphorus pesticides in olive oil

An on-line combination of gel permeation chromatography and gas chromatography has been designed using either a laboratory-built or a commercially available LC-GC apparatus to determine organophosphorus pesticides in olive oil. Gel permeation chromatography was used for sample pretreatment, viz. to separate the low-molecular-mass pesticides from the higher-molecular-mass fat constituents of the oil. A mixture of n-decane and the azeotropic mixture of ethyl acetate and cyclohexane was found to give an adequate separation between the fat and the organophosphorus pesticides. The pesticide-containing fraction, monitored by a UV detector, was transferred on-line to the gas chromatograph using a loop-type interface. n-Decane (6%, v/v) was added to the eluent in order to widen the application range of the transfer technique towards more volatile pesticides. After solvent evaporation through the solvent vapour exit and subsequent GC separation, the compounds were selectively detected with a thermionic or a flame photometric detector. The set-up allowed the direct analysis of oil samples after dilution in the gel permeation chromatography eluent without further sample clean-up. Detection limits were about 5 and 10 μg/kg with the thermionic and the flame photometric detector, respectively, when using an injection volume of only 30 μl of the 20-fold diluted oil. The total procedure was linear in the 0.01–10 mg/kg range for both detectors. For twenty organophosphorus pesticides, the relative standard deviations were 3–13% at the 20–60 μg/kg level.     

细小乳状液的制备

For preparing O/W miniemulsions containing soybean oil and silicone oil, three methods, phase inversion emulsification, D-phase emulsification, reformed D-phase emulsification were tested by using Brij92, 97, 98 and Tween 80, 85, 60, 20 and Span 80, 60 mixed surfactants. It was found that the O/W miniemulsions of soybean oil and silicone oil can not be formed by phase inversion emulsification method, but can be formed by the two other methods. The results of emulsification showed that if gel emulsion, in which fine oil droplets disperse in continuous phase with high surfactant content, appears during the emulsification process, the O/W miniemulsions can be formed by simply diluting with water.     

正化学源-气相色谱-质谱法测定食用植物油中有机锡化合物残留

建立了正化学源-气相色谱-质谱技术测定食用植物油中有机锡化合物残留的方法。食用油样品经环己烷-乙酸乙酯（1：1，v/v）溶解后，经凝胶渗透色谱（GPC）净化，目标馏分用四乙基硼酸钠进行衍生。采用基质校正曲线外标法定量，在20~2000 μg/L范围内，7种有机锡化合物均呈现良好的线性关系，相关系数大于0.99，定量限为0.3~1.2 μg/kg。对芝麻油样品进行加标回收试验，在0.05、0.10、0.20 mg/kg 3个添加水平下，7种有机锡化合物的平均回收率为66.2%~103.2%，相对标准偏差均小于11.5%。该方法精密度好，灵敏度高，可用于食用植物油中有机锡化合物残留量的测定。     

Isolation and analysis of trace level of silicone oil in pharmaceutical bulk drug substance by ICP-AES

In order to evaluate the extent of silicone oil contamination in a drug substance derived from processing equipment, a novel extraction method was developed which uses a mixture of polar and non-polar solvents (toluene/acetonitrile). Unlike the majority of silicone oil extraction methods in the literature that yield very low recoveries, this procedure proved able to completely recover the silicone oil from this compound. The recovered silicone oil was rediluted in isopropanol alcohol (IPA)/toluene mixture and subsequently analyzed by an inductively coupled plasma atomic emission spectrometer (ICP-AES) coupled to an ultrasonic nebulizer (USN).     

Proficiency test on the determination of mineral oil from polluted soils

Mineral oil products are abundant sources of environmental contamination. A Finnishproficiency test was carried out to investigate the quality of data provided in an analysis of mineral oil in polluted soils. The homogeneity and stability of the samples were tested. The calculated concentration or the median value of the results was used as the assigned value because of the unavailability of certified reference materials (CRMs). The samples were analysed using an infrared spectroscopy (IR) or gas chromatography (GC) procedure. Even if the participating laboratories had little experience with GC, the results were promising. Hence, the GC procedure will replace IR as the new ISO standard (ISO/DIS 16703) in the near future in many Finnish environmental laboratories. There is a need for CRMs for the determination of mineral oil using the GC method due to common contamination problems caused by mineral oil. Received: 9 December 2001 Accepted: 14 February 2002     

Estimation of Residual Nickel and Some Heavy Metals in Vanaspati Ghee

To convert vegetable edible oils into vanaspati ghee, nickel is used as a catalyst in the hydrogenation process. A simple and fast method for the trace level determination of nickel in ghee is reported. In this work different methods were applied for the extraction of residual nickel from ghee samples. Using toluene, benzene and carbon tetrachloride as organic solvents, an acid mixture was used for the extraction of nickel. Extracted nickel was quantified with atomic absorption and colorimetric methods. Among the organic solvents, toluene proved to be the best solvent mediating a 95% extraction of nickel from ghee samples. Nickel was extracted and determined in ten different brands of ghee and in all samples its amount was well above the permissible limit of WHO (0.2 μg/g). Other metals like lead, zinc, copper, and cadmium were also determined and their concentrations were found to be much below the WHO permissible limits.     

无溶剂体系中脂肪酶催化红花油水解反应

无溶剂体系中脂肪酶催化红花油水解反应;水解;红花油;无溶剂体系;脂肪酶     

Chemotaxonomy of aromatic plants of the genus <Emphasis Type="Italic">Origanum</Emphasis> via vibrational spectroscopy

Fourier transformed-Raman (FT-Raman) and attenuated total reflection-infrared (ATR-IR) spectra of essential oils obtained from marjoram and oregano plants by hydrodistillation are presented. It is shown that the main components of the essential oils can be ascertained through both of these complementary techniques, using spectral information from the pure terpenoids. Spectroscopic analysis is based on the characteristic key bands of the individual volatile substances and therefore, in principle, these techniques allow us to discriminate between different essential oil profiles from individual oil plants of the same species (chemotypes). The combination of vibrational spectroscopy and hierarchical cluster analysis provides a fast, easy and reliable method for chemotaxonomy characterisation. The spectroscopic data presented here correlate very well with those found by gas chromatography (GC) analysis.     

流动注射-导数火焰原子吸收光谱测定植物油中的镍、锰、铬和铅

提出了流动注射－导数火焰原子吸收光谱测定植物油中微量镍、锰、铬和铅的新方法，流动注射进样技术克服了常规火焰原子吸收法耗样量大和基体干扰严重的缺点，导数技术应用于火焰原子吸收可提高方法的灵敏度和信号的选择性，流动注射与导数技术相结合应用于火焰原子吸收成功地测定了常规火焰原子吸收法和流动注射－火焰原子吸收法难以测定的植物油中微量镍、锰、铬和铅。镍、锰、铬和铅的特征浓度（μg/mL)，分别为0.0054、0.0034、0.0067、0.025，相对标准偏差在0.3%-2.8%的范围内。     

脂肪酸量子化学特性对食用油脂生物学效应的影响

对一些食用油脂中的主要脂肪酸组份的量子化学参数进行计算，并与饲喂大鼠的相应生物学效应进行相关分析的结果表明，在各项大鼠血脂生化指标中，只有血清总胆固醇（TC）和低密度脂蛋白-胆固醇含量与脂肪酸各项量子化学参数间存在显著性相关（P＜0．05），其中单不饱和脂肪酸（MUFA）的效果优于多不饱和脂肪酸（PUFA）。MUFA还可有效降低机体丙二醛含量，增强生物膜的流动性（P＜0．01）．不饱和脂肪酸分子中烯键碳原子上量子化学参数的急剧变化是油脂产生显著生物学效应的基本条件．