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51.
IntroductionWith the improvement of living standard,people pay more and more attention to health.Theaccurate and sensitive identification ofmicroorganisms plays an important role indiagnosing disease,identifying public healthhazards from pathogens,monitoring potential foodcontamination,regulating bioprocessingoperations,and detecting or identifying the natureof biological agents[1,2 ] . There are two major goalsfor the identification of microorganisms. Onewould be to develop a method to use in… 相似文献
52.
全二维气相色谱/飞行时间质谱法在莪术挥发油组成分析中的应用 总被引:9,自引:0,他引:9
通过优化GC×GC的柱系统、温度程序和调制参数等色谱条件,建立了分析中药莪术挥发油组成的全二维气相色谱/飞行时间质谱(GC×GC/TOFMS)方法,实现了莪术挥发油的单个组分与族组分分析.采用所建立的GC×GC/TOFMS方法,鉴定出匹配度大于800的组分有249种,其中单萜18种,单萜含氧衍生物34种,倍半萜35种,倍半萜含氧衍生物37种,有69种组分的体积分数大于0.02%. 相似文献
53.
The dynamics of S(3P2,1,0; 1D2; 1S0) production from the 193 nm photodissociation of CH3SH has been examined by 2+1 resonance-enhanced-multiphoton-ionization (REMPI) techniques. Using the rate equation scheme, we have rationalized the intensities of S(3P2,1,0; 1D2; 1S0) observed according to the sequential two-photon dissociative pathways, (A): CH3SH + hv (193 nm) → CH3S + hv (193 nm) → S and (B): CH3SH + hv (193 nm) → HS + hv (193 nm) → S, as the major mechanisms for S production. We have satisfactorily fitted the photodissociation laser power dependencies for S(3P) and S(1D) produced from CH3SH by invoking photodissociation cross sections and branching ratios S(3P)/S(1D) for CH3S and HS similar to those determined previously in the 193 nm photodissociation of CH3SCH3 and H2S. This observation supports that the 193 nm photodissociation of CH3S and HS prepared from CH3SH yield predominantly S(lD) and S(3P), similar to the cases for CH3S prepared from CH3SCH3 and for HS prepared from H2S, respectively. A small amount of S(1S0) observed from the 193 nm photodissociation of CH3SH is attributed to pathway (B). 相似文献
54.
采用角分辨分子束散射技术研究了Cl_2与InP(100)表面热反应和激光诱导反应产物的角分布. 对于热反应, 由调制分子束和可转动四极质谱仪测得产物离子InCl~+、InCl_2~+、PCl~+、PCl_2~+和P_4~+的角分布, 都可用cos~(1.5)θ函数报合. 对于紫外(355 nm)激光诱导反应, 由飞行时间质谱法测得主要产物离子的角分布明显地偏离Knudsen定律. 其中In~+, InCl~+和InCl_2~+的角分布可用α·cosθ+(1-α)cos~nθ函数拟合, 其中α和n为拟合参数, 对于不同的产物离子有不同的数值. 由实验测得的脱附粒子的通量和能量在表面法线方向有明显地聚集现象, 可以认为产物从表面上脱附的机理, 除了热脱附之外, 还有非热脱附以及在表面附近脱附粒子的碰撞效应. 相似文献
55.
LI Qian-rong XUE Song YIN Hao 《高等学校化学研究》2006,22(1):40-44
IntroductionIn1893,Pietro Biginelli reported the first synthe-sis(termed the Biginelli reaction)of3,4-dihydropyrim-idinone(denoted as“oxo-orO-Biginelli compound”in-cluding its derivatives,type A in Scheme1).In thelast decade,interest in these compounds … 相似文献
56.
《Analytica chimica acta》2003,479(2):203-214
A flow injection (FI) method was developed using electrochemical hydride generation (EcHG) as a sample introduction system, coupled to an inductively coupled plasma time-of-flight mass spectrometer (ICP-TOFMS) for rapid and simultaneous determination of six elements forming hydrides (As, Bi, Ge, Hg, Sb and Se). A novel low volume electrolysis cell, especially suited for FI experiments was designed and the conditions for simultaneous electrochemical hydride generation (EcHG; electrolyte concentrations and flow rates, electrolysis voltage and current) as well as the ICP-TOFMS operational parameters (carrier gas flow rate, modulation pulse width (MPW)) for the simultaneous determination of 12 isotopes were optimized. The compromise operation parameters of the electrolysis were found to be 1.4 and 3 ml min−1 for the anolyte and catholyte flow rates, respectively, using 2 M sulphuric acid. An optimum electrolysis current of 0.7 A (16 V) and an argon carrier gas flow rate of 0.91 l min−1 were chosen. A modulation pulse width of 5 μs, which influences the sensitivity through the amount of ions being collected by the MS per single analytical cycle, provided optimum results for the detection of transient signals. The achieved detection limits were compared with those obtained by using FI in combination with conventional nebulization (FI-ICP-TOFMS); values for chemical hydride generation (FI-CHG-ICP-TOFMS) were taken from the literature. By using a 200 μl sample loop absolute detection limits (3σ) in the range of 10-160 pg for As, Bi, Ge, Hg, Sb and 1.1 ng for Se and a precision of 4-8% for seven replicate injections of 20-100 ng ml−1 multielemental sample solutions were achieved. The analysis of a standard reference material (SRM) 1643d (NIST, “Trace Elements in Water”) showed good agreement with the certified values for As and Sb. Se showed a drastic difference, which is probably due to the presence of hydride-inactive Se species in the sample. Recoveries better than 93% for Ge and Hg and 83.9% for Se were achieved on a spiked SRM sample. The developed method was successfully applied to the simultaneous multielemental determination of hydride forming elements in spring water samples originating from two different regions in Hungary. 相似文献
57.
First, standard mixtures of trimethylsilyl (TMS) derivatives of amino acid and organic acid are analyzed by comprehensive two-dimensional (2D) gas chromatography (GC) coupled to time-of-flight mass spectrometry (GC × GC/TOFMS) in order to illustrate important issues regarding application of the technique. Specifically of interest is the extent to which the peak capacity of the 2D separation space has been utilized and the procedure by which the derivative standards are identified in the 2D separations using the mass spectral information. The resulting 2D separation is found to make extensive use of the GC × GC separation space provided by the complementary stationary phases employed.Second, in order to demonstrate GC × GC/TOFMS on two real sample types, trimethylsilyl metabolite derivatives were analyzed from extracts of common lawn grass samples (i.e., perennial rye grass), as a means to provide insight into both the pre and post harvest physiology. Various chemical components in the two rye grass extract samples were found to either emerge or disappear in relation to the trauma response. For example, a significant difference in the peak for the TMS derivative of malic acid was found. The successful analysis of various components was readily facilitated by the 2D separation, while a 1D separation would have produced too much peak overlap, thus impeding the analysis. The importance of using a GC × GC separation approach for the analysis of complex samples, such as metabolite extracts, is therefore demonstrated. The real-time analysis capability of GC × GC/TOFMS for multidimensional metabolite analysis makes this technique well suited to the high-throughput analysis of metabolomic samples, especially compared to slower, stopped-flow type separation approaches. 相似文献
58.
Neutral benzene-ammonia clusters, prepared in a supersonic expansion, were ionized using multiphoton ionization. The cluster ions were investigated with a time-of-flight mass spectrometer. The observed major cluster ions, under 355-nm laser irradiation, resulting from prompt intracluster ion-molecule reaction and fragmentation following ionization are (C6H6)m(NH3)nH+, m = 1–6, n = 1–4 and (C6H6)m+, m = 1–3. The results of isotopic labeling experiments clearly indicate that C6H6 does not participate in intracluster ion-molecule reactions to form (C6H6)m(NH3)nH+. A local maximum appears at n = 2 in the intensity distribution of (C6H6)m(NH3) nH+ for each value of m under all experimental conditions. This finding indicates that (C6H6)m(NH3)2H+ is more stable than any other (C6H5)m(NH3)mH+ (n = 1,3,4) for m = 1–6. 相似文献
59.
G. Du H.Y. Zhao Q.W. Zhang G.H. Li F.Q. Yang Y. Wang Y.C. Li Y.T. Wang 《Journal of chromatography. A》2010,1217(5):705-714
A microwave-assisted extraction (MAE) and ultra high performance liquid chromatography coupled with diode array detection and time-of-flight mass spectrometry (UHPLC-DAD-TOF-MS) method was developed for simultaneous determination of 14 phenolic compounds in the root of Pueraria lobata (Wild.) Ohwi and Pueraria thomsonii Benth. Operational conditions of MAE were optimized by central composite design (CCD). The optimized result was 65% ethanol as extraction solvent, 17 mL of extraction volume, 100 °C of extraction temperature and 2 min of hold time. A Zorbax SB C18 (50 mm × 4.6 mm I.D., 1.8 μm) and gradient elution were used during the analysis. The chromatographic peaks of 14 investigated compounds in samples were successfully identified by comparing their retention time, UV spectra and TOF mass data with the reference substances. All calibration curves showed good linearity (r > 0.9997) within the test ranges. The intra-day and inter-day variations were less than 1.77% and 2.88%, respectively. The developed method was successfully applied to determine the investigated compounds in 10 samples of Radix Puerariae Lobatae and Radix Puerariae Thomsonii, respectively. The result indicated that MAE and UHPLC-DAD-TOF-MS system might provide a rapid method for the quality control of Radix Puerariae. 相似文献
60.
Aline Staub Serge Rudaz Jean-Luc Veuthey Julie Schappler 《Journal of chromatography. A》2010,1217(51):8041-8047
This paper describes an efficient CE-UV-ESI-TOF/MS method for the determination and quantitation of intact insulin (INS) in a pharmaceutical formulation. The CE conditions were optimized to avoid the adsorption of proteins onto the capillary wall. Particular attention was paid regarding the choice of the internal standard (IS). A strategy based on multiple injections was selected and the methodology was validated according to international guidelines. The optimized method was applied with success to the analysis of INS formulations obtained from regular and parallel markets. 相似文献