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1.
Reference proteinaceous binding media of the kinds historically used in painting (specially prepared for this study) and
samples collected from ancient polychrome works of art were analysed by gas chromatography – mass spectrometry. The data have
been processed by several multivariate chemometric techniques, such as cluster analysis, principal component analysis, factor
analysis and SIMCA technique in order to classify the binding media of the ancient works of art on the basis of the proteinaceous
material used. The characterisation of ancient samples was possible by the joint use of SIMCA technique and factor analysis.
The latter, in particular, has made it possible to point into evidence the presence of at least two latent factors. The first
factor seems to be connected with the chemical composition of the painting media, while the second factor is likely to be
connected with ageing processes.
Received: 14 October 1998 / Revised: 23 April 1999 / Accepted: 20 May 1999 相似文献
3.
报道了调味品中氯丙醇的衍生化气相色谱(GC/ECD)和衍生化气相色谱双串联质谱法(GC/MS/MS)测定。GC/ECD测定酱油中3—氯—1,2—丙二醇(3—MCPD)的检出限达到0.01mg/kg,回收率为91%~104%,变异系数为2.27%~7.96%;GC/MS/MS同时测定酱油中1,3—二氯—2—丙醇、2,3—二氯—1—丙醇和3—氯—1,2—丙二醇,1,3—二氯—2—丙醇、2,3—二氯—1—丙醇的检出限为0.02mg/kg,3—氯—1,2—丙二醇的检出限为0.01mg/kg,回收率在92%~106%,变异系数为3.51%~13.33%。 相似文献
4.
研究了用气相色谱-质谱分析化妆品中氯霉素(CAP)的方法.以乙酸乙酯作为提取溶剂,BSTFA TMCS(99 1)作为衍生化试剂,在70℃衍生化60min,用GC-MS(NCI)进行测定.方法的检出限为10 μg/kg,线性范围在0.5~500 ng/mL之间,在10、100、500 μg/kg 3个添加水平,方法回收率为94.4%~95.7%,相对标准偏差为0.23%~1.3%.方法操作快速简单,3 h可以完成整个样品分析.方法已用于化妆品中氯霉素的测定. 相似文献
5.
Ion mobility spectrometry (IMS) is a well-known analytical method for the detection of CWAs and explosives since many years. Coupling IMS to GC pre-separation, new application fields in medicine and biology could be opened, dealing with complex and humid mixtures. However, identification of unknowns in such a complex sample is challenging and can only be achieved by parallel GC/MS analysis, thus obtaining a proposal for the responsible compound for validation via reference substances by GC/IMS again. The available adsorption tools for such accompanying GC/MS analysis have their particular drawbacks (e.g. problematic quantification for SPME, high sample volumes for adsorption tubes). Therefore miniaturised adsorption needles (NeedleTrap) were applied to both GC/IMS and GC/MS for validation of their reproducibility. It could be demonstrated that the needles can even be used for appropriate quantification when the adsorbent and the sample volume are adapted properly to the concentration range, the compounds of interest and humidity of the sample. The method is very flexible with regard to the concentration range by variation of the sample volume (e.g. 20 mL for ppt V, 10 mL for lower ppb V or 1 mL for ppm V) and with regard to the compounds of interest by application of common adsorption materials optimised for the relevant substance group. Such materials are available commercially in a broad variability. Therefore, the miniaturised adsorption needles are a helpful complementary sampling method for any GC/MS or GC/IMS investigations. 相似文献
6.
Analytical methods have been developed that allow for the determination of antiphlogistics, lipid regulators, the antiepileptic carbamazepine, cytostatic agents, the psychiatric drug diazepam and iodinated contrast media (ICM) as well as two major polycyclic musk fragrances HHCB (galaxolide) and AHTN (tonalide) in activated and digested sludge. The procedures consist of ultrasonic solvent extraction (USE) using methanol/acetone or pressurized liquid extraction (PLE) using 100% methanol. Clean-up was performed with C18ec material and silica gel followed by LC tandem MS (electrospray or atmospheric pressure chemical ionization) detection for pharmaceuticals and iodinated contrast media as well as GC/MS in the SIM mode for musk fragrances. Absolute recoveries from spiked activated sludge in general ranged from 88+/-4 to 119+/-20% for ICM and were 78+/-15 and 87+/-10% for the AHTN and HHCB, respectively. For the pharmaceuticals, absolute recoveries in activated sludge ranged between 43 and 78%. Subsequently, compensation of losses was carried out by using surrogate standards (acidic pharmaceuticals: fenoprop, neutral pharmaceuticals: dihydro-carbamazepine, musk fragrances: AHTN-D3). With one exception the recoveries were also adequate in digested sludge ranging from 43% to 120%. 相似文献
7.
多廿醇是从制糖滤泥中分离得到的一种高级脂肪伯醇天然混合物,其化学组成分析未见报道。本文采用气相色谱法(GC)和气相色谱/质谱法(GC/MS),对其组分和结构进行了分析和鉴定。 相似文献
8.
本文用毛细管GC/MS和GC/FTIR对异叶青兰和鼠曲草两种植物挥发油的化学成分进行了研究,讨论了两种方法分析挥发油化学成分的优点和局限性。 相似文献
11.
Polycyclic aromatic hydrocarbons (PAHs), apart from their carcinogenic and mutagenic nature, create many problems in the petrochemical industry due to their tendency toward carbonization. Compounds in C8 aromatic isomer feed are analyzed by means of sample concentration, followed by separation of individual compounds by gas chromatography on a stainless steel OV-101 phase capillary column and identification by gas chromatography/mass spectrometry and gas chromatography/Fourier transform infrared spectroscopy. Various compounds belonging to different classes (mainly monocyclic, dicyclic, and tricyclic aromatics), oxygenated aromatics, and aliphatic saturates are quantified in the concentrated hydrocarbon residue of C8 isomer feed. Both unsubstituted and alkyl substituted ring type compounds are present. Concentrations obtained for PAH compounds in the C8 isomer feed range from 0.2 to 0.42 micrograms/mL. 相似文献
14.
A rapid extraction procedure for fingerprint chromatogram of different types of Mentha piperita L. (Labiatae family) is presented. The extracts were analysed by gas chromatography and gas chromatography-mass spectrometry (GC/MS). The main volatile compounds identified by the gas chromatography-mass spectrometric analysis of M. piperita L. were menthol, menthone, isomenthone, 1,8-cineole, menthyl acetate, limonene, beta-myrcene, carvone. M. piperita L. oil had the active principles: menthol, menthone, isomenthone, menthyl acetate, alpha-pinene, beta-pinene, champhor, limonene, linalool, piperitone. M. crispa L. showed carvone as major component. 相似文献
15.
The concentrations of nandrolone metabolites, 19-norandrosterone (19-NA) and 19-noretiocholanolone (19-NE) were analysed in urine samples of professional athletes doing intense physical activity and sedentary subjects to verify if there was endogenous production of nandrolone and if there was any link between physical effort and the urinary metabolites of the steroid. We collected 18 urine samples from professional footballers age range 20-30 years, all from the same team, and 18 urine samples from males not doing any physical activity, age range 20-30 years. Neither group used nandrolone. Qualitative and quantitative analyses of urinary nandrolone metabolites were carried out by GC/MS followed by GC/MS/MS to confirm positive samples. This technique has been demonstrated to be an excellent analytical approach for the determination of anabolic steroids at very low detection limits in complex matrices such as urine. In five urine samples from professional footballers traces of 19-NA were detected. No trace of 19-NA was found in the group of sedentary subjects and no trace of 19-NE was found in any urine sample. The absence of nandrolone metabolites in sedentary subjects supports the hypothesis that the presence of 19-NA and 19-NE could be linked to physical effort even though the origin is not yet clear. 相似文献
16.
Moscow University Chemistry Bulletin - A monolith based on foamed graphite is used for the sorption of hydrocarbons (alkanes, cycloalkanes, arenes) as markers of oil pollution. This material is... 相似文献
19.
A GC and IR based protocol was developed for monitoring the isobutene dimerisation process wherein the complete characterisation of the products was carried out by GC coupled with mass spectrometry. In the dimerisation process, LPG from FCC process comprising a mixture of saturated and unsaturated C4 hydrocarbons is subjected to a dimerisation process using a catalyst to produce C8 hydrocarbons. The reaction is carried out keeping in view the demand for high-octane blending components in gasoline. The isooctene generated in the process (mainly from the dimerisation of isobutene) is converted into isooctane having the RON and MON value 100. The monitoring process requires the use of two different column chemistries, viz., a 100 m CPSIL PONA CB non-polar column for C8 and its isomers and an Alumina PLOT column for C4 hydrocarbons. A 100 m non-polar column does not separate the C4 mixture since the column is meant for gasoline range products containing C5 and above hydrocarbons. Therefore, a need was felt for an improvised method which can handle both the analyses simultaneously. A cryogenic oven program starting from 0 °C was developed for separating the isomers of C4 hydrocarbons and C8 hydrocarbons on a single column during the single run by Detailed Hydrocarbon Analyzer. The data obtained using the cryo programme was validated with data obtained using Alumina PLOT column on C4 mixture since the Alumina PLOT column is the widely accepted column chemistry for separating the C4 hydrocarbons. An IR method for the estimation of the total olefin content was developed using 2,2,4-trimethyl pentene-1 as the reference standard. The total olefins generated during the process were identified by GC–MS, quantified by DHA-FID and validated by infrared spectroscopy. A good correlation was found between GC and IR spectral results (correlation coefficient R
2 = 0.99). 相似文献
20.
The essential oil composition of the flowers of Senecio belgaumensis (Wight) Cl. was analyzed by gas chromatography and gas chromatography/mass spectrometry. Forty eight compounds were identified, representing 91.5% of the total oil. The main constituents were 1-undecanol (19.5%), beta-caryophyllene (18.9%), caryophyllene oxide (10.4%) and y-terpinene (9.2%). 相似文献
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