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991.
Fast gas chromatography/negative-ion chemical ionization mass spectrometric (GC/NICI-MS) assay combined with rapid and nonlaborious sample preparation is presented for the simultaneous determination of benzodiazepines and alpha-hydroxy metabolites, zaleplon and zopiclone in whole blood. The compounds were extracted from 100 microl of whole blood by simultaneous multitube, microscale liquid-liquid extraction (LLE) and derivatized by N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide (MTBSTFA), without the need for the time-consuming concentration stage. In the analytical separation, various parameters of fast GC/NICI-MS were applied, e.g. the use of hydrogen as a GC carrier gas, a high carrier gas velocity, a small film thickness of the analytical column, fast MS data acquisition, fast temperature ramping, and high initial and final temperatures of GC column. Sensitive identification, screening and quantitation of 18 compounds of interest were achieved in chromatographic separation in only 4.40 min. Accurate and reproducible results were obtained by using five different and carefully selected deuterated analogues on the basis of the chemical properties of the target analytes. Nevertheless, for alpha-OH-midazolam, and for bromazepam and flunitrazepam at low concentrations, the results can be considered only semiquantitative on the basis of the validation data. The extraction efficiencies ranged from 74.3 to 105.7% and the limits of quantitation (LOQ) from 1 to 100 ng ml(-1). Rapid sample preparation and fast chromatographic separation allowed cost-efficient, reliable and high sample-throughput analyses with a low amount of manual work. The method was fully validated and accredited according to EN ISO/IEC 17025 standards and is applicable for sensitive, reliable and quantitative determination of benzodiazepines, zaleplon and zopiclone, e.g. in clinical and forensic toxicology. 相似文献
992.
常压下以内循环无梯度反应器研究了B108铁基中温变换催化剂上水煤气变换反应宏观动力学。测定了反应速率,并用马夸特非线性参数估值法获得了幂函数宏观动力学模型r_s=37.67exp(-43982/RT)y_(CO)~(0.7552)y_(H_2O)~(-0.0367)Y_(CO_2)~(-0.4874)y_(H_2)(1-β)根据方差分析和残差分析,证实模型是高度显著的。由实验数据计算出相应反应条件下的效率因子。内扩散对原粒度B108催化剂上的反应具有严重影响。模型用于工业变换炉催化剂的用量核算,模型值与实际值符合良好。 相似文献
993.
994.
Bio-, thermo-catalytic transitional zone gas (BTCTZ gas), of which burial depth is shallow (1000-2500m), chemical composition (C,/ΣC1-5 = 0.7-0.9) and isotopic composition (δ13C1= -55 to-48‰) coincide with the evolution level of organic matter (R0=0.25-0.6%) in the corresponding strata, is a natural gas of new genetic type. The genesis of BTCTZ gas must have some relation to microcatalysis under lower temperature and condensation of aromatic hydrocarbons. In line with the new theory of natural gas formation, the existence of BTCTZ gas is objective. According to data from all over the world, BTCTZ gas may hold an important position in the table of reserves of natural gas. 相似文献
995.
研究了三甲基硅烷基丙块与五甲基二硅烷基丙块共聚物〔poly(TMSP-co-PMDSP)〕的成膜特点。poly(TMSP-co-PMDSP)膜的气体透过系数分别为:P_(O2):4×10~3~12×10~3,P_(N2):3×10~3~8×10~3和P_(CO2):2×10~4~4×10~4barrer,气体透过稳定性低,透过行为偏离第二Fick定律,过系数下降,其中溶解系数降低的比例远大于扩散系数的增加比例,在含有凝聚性气体的环境里,膜的气体透过出现表面吸附控制的特征。 相似文献
996.
997.
Gencai Cai 《Journal of Thermal Analysis and Calorimetry》1995,45(1-2):167-176
An established DTA/T/EGD/GC on-line coupled simultaneous technique and relevant equipment were applied to identify the micro impurity minerals—pyrite and siderite in two kinds of dolomite in air and N2. The proportional five-component mixed minerals (siderite, kaolinite, dolomite, calcite and quartz) and the proportional six-component mixed minerals (pyrite and the above five minerals) were detected in N2 and in air/CO2 (1∶1) separately by applying DTA/EGD/GC and DTA/GC. The experimental results provide the basis for demonstration of the reaction mechanism of thermal decomposition of various gas—solid-phase minerals in N2 and air/CO2. The compositions of six-component mixed minerals can be distinguished individually from the DTA/GC curves; reliable results are obtained. 相似文献
998.
999.
毛细管气相色谱法测定热不稳定有机磷农药辛硫磷 总被引:11,自引:0,他引:11
The thermo-labile organophosphorous pesticide Phoxim was determined by capillary gas chromatographywith flame phototnetric detector. When high linear velocity H_2(>200cm/s) was used as carrier gas,the thermo-decomposition of Phoxim was considerably reduced.The most important gas chromatography conditions,injectortempereture and column head pressure,were studied.The thermo-decomposition preducts were identified by gaschromatography-mass spectrometry. 相似文献
1000.