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1.
微波消解同时衍生化GC—MS法测定血浆中脂肪酸的研究   总被引:5,自引:0,他引:5  
研究了利用微波能对样品进行加热,以H2SO4-甲苯-甲醇体系作衍生化试剂,在消化的同时对血浆中的脂肪酸进行衍生化,然后用GC-MS法测定血浆中脂肪酸。对微波功率、微波加热时间、消解及衍生化试剂等条件进行了优化,测定结果较好。该法整个消化及衍生化过程只需2min,与传统方法相比大大缩短了实验操作时间,特别适用于大量样品的测定。  相似文献   

2.
微波消解同时衍生化GC-MS法测定血浆中脂肪酸的研究   总被引:3,自引:0,他引:3  
研究了利用微波能对样品进行加热, 以H2SO4 - 甲苯- 甲醇体系作衍生化试剂, 在消化的同时对血浆中的脂肪酸进行衍生化, 然后用GC- MS 法测定血浆中脂肪酸。 对微波功率、微波加热时间、消解及衍生化试剂等条件进行了优化, 测定结果较好。该法整个消化及衍生化过程只需2 min , 与传统方法相比大大缩短了实验操作时间, 特别适用于大量样品的测定。  相似文献   

3.
低碳醇合成中异丁醇形成机理及提高其收率的途径   总被引:4,自引:4,他引:4  
在压力10MPa,温度360~420℃,尾气空速3000~7000h ̄(-1)的反应条件下,采用分别富集甲醇、乙醇、正丙醇和异丙醇的方法,研究Zn-Cr-K氧化物催化剂上异丁醇的形成机理,并探讨利用甲醇循环提高其收率的可能性。结果表明,低碳醇的形成是以碳链增长形式进行的,COH→CCOoH慢的α-加成反应是链增长的起始步骤,也是低碳醇合成反应的控制步骤,β-加成是生成低碳醇的特征反应,COH→CCOH→CCCOH→CC(CH_3)COH是异丁醇的形成机理。甲醇富集对提高异丁醇收率有明显的促进作用,采用甲醇循环技术提高异丁醇收率是可行的。  相似文献   

4.
旋光活性○-乙基-○-苯基硫代磷酰胺酯在4.7mol/L HCl-MeOH溶液中进行酸性甲醇解时得到P-N键断裂的构型翻转产物,与MeONa-MeOH的碱性甲醇解得到以PhO基为离去基的构型翻转产物。两种甲醇解反应的机理均可用三角双锥(TBP)中间体概念完满地解释。  相似文献   

5.
朱兵  汪仁 《燃料化学学报》1997,25(5):445-448
利用原位红外技术研究了CH3OH,CO,O2等在Pd/γ-Al2O3上的吸附情况及CH3OH和O2共吸附时表面物种的变化,结果表明,表面纯净的Pd/γ-Al2O3催化剂对甲醇具有很好的解离吸附性能,在无氧条件下,CH3OH可在其上脱氢产生HCHO及CO。Pd对O2的吸附力强,氧均以解离方式吸附于Pd/γ-Al2O3上。当吸附的「CH3O」与「O」的Pd/γ-Al2O3上相互作用时,可产生HCHO,  相似文献   

6.
硬脂酸镍L—B膜对甲醇的电催化氧化   总被引:1,自引:0,他引:1  
华炳增  张韫宏 《电化学》1997,3(3):282-286
硬脂酸镍L-B膜电极对甲醇具有良好的电催化作用,膜中镍离子主要以-CooNi(OH)形式存在,电催化过程受OH-浓度的影响,也涉及甲醇分子在膜内的穿透。  相似文献   

7.
双模板剂法控制SAPO-34分子筛的晶粒尺寸   总被引:2,自引:0,他引:2  
分别在NEt_3,TEAOH和TEAOH-NEt_3双模板剂存在下合成了磷酸硅铝分子筛SAPO-34.考察了模板剂的组成对SAPO-34的晶粒尺寸、比表面、热稳定性和对甲醇转化反应催化性能的影响。实验表明,采用TEAOH-NEt_3双模板剂法,能有效地控制SAPO-34的晶粒尺寸,以微量的TEAOH与NEt_3为双模板剂合成的大晶粒SAPO-34分子筛,对甲醇转化产物和烯烃的选择性有显著提高  相似文献   

8.
分别以清洁及氧悠Cu(100)表面作为金属态铜和部分氧化态铜的表面模拟,用键级守恒-Mores势法研究了两种表面上CO2加氢制甲醇反应的能量学,计算结果表明,在两种表面上,CO2加氢制甲醇反应的优势反应途径均为“CO2,s→HCOOs→H2COs→CH3Os→CH3OHs”与清洁铜表面上的相应基元步骤相比,在Cu(100)-p(2×2)O表面上甲醇合成反应各基元步骤具有更低的活化能;HCOOs是含  相似文献   

9.
制备了Cu-Zn-Al (4/50/5)催化剂(Cat)和Cu-Zn-Al-Li(40/50/5/5)催化剂(Cat-Li).并将其分别用于由CO/H_2和CO_2/H_2合成甲醇。诸如TPD、TPR、TPSR、脉冲、CD3I-捕获、同位素标记、EPR及原位DRIFT等技术和方法被用来表征这两种催化剂及研究反应机理,对处于去氢、含氢及含氧态催化剂进行了对比研究以期阐明表面氧和表面氢对CO_2和CO活化所起的作用。提出了一个由甲酸根和甲醛氢化及甲醇氧化结果为证的CO/CO_2氢化机理。由于通过Li 取代CuO晶格上的Cu2+形成的氢空位,在Cat中添加Li+改善了甲醇合成活性。CO_2能被一捕获的电子(F-中心)活化,生成的CO2-能容易地被氢化成甲酸根和亚甲基双草酰,后者分解生成H2CO和表面氧。CO能被表面氧活化,生成的CO2-将遵循CO_2氢化的途径。在CD3I-捕获的实验中,我们捕获了表面氧。在无表面氧时,CO可能直接氢化成甲酸基,即CO_2氢化中的一途径。由亚甲基双草酰产生的H2CO表面模型可能与由甲醛吸附或CO氢化生成的H2CO表面模型不同。  相似文献   

10.
采用半微量相平衡方法研究了三元体系Y(ClO4)3.3H2O-B15C5-CH3OH在25℃的溶解度,测定了各饱和溶液的折光率。该体系在25℃生成三种化学计量的配合物,其组成分别为:4Y(ClO4)3.3B15C5.12H2O.12Ch3OH(I),Y(ClO4)3.2B12C5.3H2O.Ch3OH(Ⅲ),其中配合物(I)和(Ⅱ)是溶解不一致化合物。在甲醇溶剂中,分离制备了配合物(Ⅲ),在69-  相似文献   

11.
Xu X  Su R  Zhao X  Liu Z  Zhang Y  Li D  Li X  Zhang H  Wang Z 《Analytica chimica acta》2011,707(1-2):92-99
The ionic liquid-based microwave-assisted dispersive liquid-liquid microextraction (IL-based MADLLME) and derivatization was applied for the pretreatment of six sulfonamides (SAs) prior to the determination by high-performance liquid chromatography (HPLC). By adding methanol (disperser), fluorescamine solution (derivatization reagent) and ionic liquid (extraction solvent) into sample, extraction, derivatization, and preconcentration were continuously performed. Several experimental parameters, such as the type and volume of extraction solvent, the type and volume of disperser, amount of derivatization reagent, microwave power, microwave irradiation time, pH of sample solution, and ionic strength were investigated and optimized. When the microwave power was 240 W, the analytes could be derivatized and extracted simultaneously within 90 s. The proposed method was applied to the analysis of river water, honey, milk, and pig plasma samples, and the recoveries of analytes obtained were in the range of 95.0-110.8, 95.4-106.3, 95.0-108.3, and 95.7-107.7, respectively. The relative standard deviations varied between 1.5% and 7.3% (n=5). The results showed that the proposed method was a rapid, convenient and feasible method for the determination of SAs in liquid samples.  相似文献   

12.
A rapid and cost‐effective method based on microwave‐assisted extraction followed by capillary electrophoresis was developed for simultaneous quantification of seven alkaloids in Corydalis decumbens for the first time. The main parameters affecting microwave‐assisted extraction and capillary electrophoresis separation were investigated and optimized. The optimal microwave‐assisted extraction was performed at 40°C for 5 min using methanol/water (90:10, v/v) as the extracting solvent. Electrophoretic separation was achieved within 15 min using an uncoated fused‐silica capillary (50 μm internal diameter and 27.7 cm effective length) and a 500 mM Tris buffer containing 45% v/v methanol (titrated to pH* 2.86 with H3PO4). The developed method was successfully applied to the quantification of seven alkaloids in Corydalis decumbens obtained from different regions of China. The combination of microwave‐assisted extraction with capillary electrophoresis was an effective method for the rapid analysis of the alkaloids in Corydalis decumbens .  相似文献   

13.
李攻科  何小青  张展霞 《色谱》2000,18(4):337-339
 研究了用微波技术消解衍生化气相色谱 质谱法 (GC MS)快速测定鲨鱼软骨中脂肪酸的分析方法。用正交设计试验优化消解衍生化条件 ,以盐酸 甲醇 (体积比为 1∶4)体系作消解衍生化溶液 ,在 60 0W微波功率作用下加热 4min进行样品的前处理 ,将样品的消解、脂肪酸的衍生化及脂肪酸甲酯的萃取融于一体。方法具有灵敏度高、省时、省试剂、操作方便等特点。该法适用于大批量固体样品中脂肪酸的测定。  相似文献   

14.
A green and simple method, ionic liquid‐based microwave‐assisted surfactant‐improved dispersive liquid–liquid microextraction and derivatization was developed for the determination of aminoglycosides in milk samples. Nonionic surfactant Triton X‐100 and ionic liquid 1‐hexyl‐3‐methylimidazolium hexafluorophosphate were used as the disperser and extraction solvent, respectively. Extraction, preconcentration, and derivatization of aminoglycosides were carried out in a single step. Several experimental parameters, including type and volume of extraction solvent, type and concentration of surfactant, microwave power and irradiation time, concentration of derivatization reagent, and pH value and volume of buffer were investigated and optimized. Under the optimum experimental conditions, the linearities for determining the analytes were in the range 0.4–10.0 ng/mL for tobramycin, 1.0–25.0 ng/mL for neomycin, and 2.0–50.0 ng/mL for gentamicin, with the correlation coefficients ranging from 0.9991 to 0.9998. The LODs for the analytes were between 0.11 and 0.50 ng/mL. The present method was applied to the analysis of different milk samples, and the recoveries of aminoglycosides obtained were in the range 96.4–105.4% with the RSDs lower than 5.5%. The results showed that the present method was a rapid, convenient, and environmentally friendly method for the determination of aminoglycosides in milk samples.  相似文献   

15.
Berberine is one of the most important bioactive compounds used in Chinese herbal drugs to evaluate the quality of the Phellodendron cortex. The cortices of Phellodendron wilsonii and Phellodendron amurense, extracted by using a microwave‐assisted process under a domestic microwave oven in methanol solvent and analyzed by capillary electrophoresis with the buffer solution of 82% 0.1 M aqueous sodium acetate and 18% MeOH (v/v), were demonstrated to be higher in extracting berberine contents and shorter in the process time than those extracted by using a reflux extraction in methanol solvent (for sample B, 2.27 ± 0.08% in 3 min vs. 1.92 ± 0.14% in 5 hrs, respectively). Therefore, the microwave‐assisted process for extraction of berberine is more efficient, rapid and convenient than the reflux extraction and can be used for the extraction of bioactive substances from the crude Chinese drugs.  相似文献   

16.
In this study, a rapid and sensitive method is described for the catecholamines detection in rat brain. CE with LIF detection for the determination of FITC derivatized catecholamines (dopamine, epinephrine, and norepinephrine) was demonstrated. Conventional water bath and microwave‐assisted derivatization methods were employed and a significant reduction in the derivatization time from 2 h for the conventional water bath at room temperature (ca. 25°C) to 2 min for the microwave‐assisted derivatization was achieved. Online sample concentration of field‐amplified sample stacking (FASS) method was employed to achieve higher sensitivities (the detection limits obtained in the normal injection mode ranged from 2.6 to 4.5 ng L?1 and in the FASS mode ranged from 22 to 34 pg L?1). Furthermore, this microwave‐assisted derivatization CE–LIF method successfully determined catecholamines in rat brain with as low as 100 ng L?1 (FASS mode) to 10 μg L?1 (normal injection mode). This CE–LIF method provided better detection ability when compared to the best reports on catecholamines analyses.  相似文献   

17.
In this study, an enantioselective analytical method based on microwave‐assisted chiral derivatization coupled with ultra high performance liquid chromatography and tandem mass spectrometry was developed for the determination of bambuterol enantiomers in human plasma. The chiral derivatization reaction was greatly accelerated by microwave irradiation. Under the optimized conditions, both the derivatization time and separation time on column was only 3 min, and the lower limit of quantification was 2.5 pg/mL. The recoveries were in the range of 90.1–93.0% without significant matrix effect. Compared with the conventional heating chiral derivatization, microwave‐assisted chiral derivatization obtained higher chiral derivatization yields with much shorter time due to the effect of microwave irradiation. Furthermore, the racemization during the derivatization reaction was systematically investigated. The results showed the concentration of acetic acid and the reaction time had significant effects on the racemization, which could be well controlled during microwave‐assisted chiral derivatization for the short reaction time. Finally, this novel approach was demonstrated by determining bambuterol in human plasma of a clinical pharmacokinetic study in eight healthy volunteers. On the basis of the results, microwave‐assisted chiral derivatization coupled with ultra high performance liquid chromatography and tandem mass spectrometry as a simple and effective enantioselective analysis technique for the determination of chiral drugs in complex biological samples showed great promise.  相似文献   

18.
Microwave-assisted multi-component synthesis of fused 3-aminoimidazoles   总被引:1,自引:0,他引:1  
A variety of fused 3-aminoimidazoles have been synthesised by a microwave assisted Ugi three-component coupling (3cc) reaction catalysed by scandium triflate in methanol as solvent. Yields of 33-93% have been achieved after just 10 min of microwave irradiation using a simple one-stage procedure. The methodology described is suitable for the rapid and efficient synthesis of a range of fused heterocycles of pharmacological interest.  相似文献   

19.
Xu X  Zhao X  Zhang Y  Li D  Su R  Yang Q  Li X  Zhang H  Zhang H  Wang Z 《Journal of separation science》2011,34(12):1455-1462
A new microwave-accelerated derivatization method was developed for rapid determination of 13 natural sex hormones in feeds. Sex hormones were isolated from the sample matrix by ultrasonic extraction, followed by solid-phase extraction, derivatized under microwave irradiation, and then analyzed directly by gas chromatography-mass spectrometry (GC-MS) in selective ion monitoring (SIM) mode. The key parameters affecting derivatization efficiency, including microwave irradiation time, microwave power, and reaction solvent were studied. Under microwave power of 360 W and microwave irradiation for 3 min, 13 natural sex hormones were simultaneously derivatized using heptafluorobutyric acid anhydride (HFBA) as derivatization reagent. This method was applied to the determination of 13 natural sex hormones in different feed samples, and the obtained results were compared with those obtained by the traditional thermal derivatization. The recoveries from 58.1 to 111% were obtained at sex hormone concentrations of 10-300 μg/kg with RSDs ≤12.0%. The results showed that the proposed method was fast, simple, efficient and can be applied to the determination of 13 natural sex hormones in different feed samples.  相似文献   

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