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1.
研究了致幻性安非它明类药物MDMA和MDA的三氟乙酰、二氯乙酰、一氯二氟乙酰、五氟丙酰、七氟丁酰、五氟苯甲酰和二硝基苯甲酰衍生化的反应条件,发现所研究的各种衍生化反应均可用少量酸酐或酰氯在环已烷中室温下几分钟内完成.在此基础上建立了尿中MDMA和MDA的用微量环已烷提取的、各种衍生化的、电子俘获检测的气相色谱分析方法.方法操作简便快速,多数方法的检出限低于10μg/L,检测MDMA最灵敏的方法是七氟丁酰衍生化方法,检出限为4.1μg/L,检测MDA最灵敏的方法是五氟苯甲酰衍生化方法,检出限为2.5μg/L.对其中几种灵敏度较高的方法进行了线性关系和回收率的考查.  相似文献   

2.
本文报道了19种蛋白质氨基酸的七氟丁酰正丁酯衍生物的GC/MS分析方法;优选了衍生反应条件;建立了GC分离、定量分析方法,最小检测量为0.1ng;研究了衍生物的EI质谱数据,确定了可作为定性依据的特征离子;测定了儿童用复方氨基酸注射液及儿童血清样品,得到了满意的结果。  相似文献   

3.
对高效镇痛药盐酸二氢埃托啡的衍生化条件、色谱及质谱行为进行了研究。通过对不同衍生化试剂、衍生化反应温度、反应时间等条件的优化,选择七氟丁酰咪唑与二氢埃托啡在室温反应5min,即可生成较完全的单取代七氟丁酰衍生物。该衍生物具有较好的气相色谱和电子轰击质谱行为。其单取代分子离子的质量数为m/z609,基峰离子为m/z522,主要碎片离子分别为m/z508、534和576,并对这些离子的产生进行了解析。这些离子均有较强的相对丰度,可作为微量二氢埃托啡的多离子选择定性。而基峰离子m/z522作为其特征离子,可用于微量二氢埃托啡的单离子选择定量。最低检测限为1pg。  相似文献   

4.
赵冰  谭家镒  姜兆林  姚丽娟 《分析化学》2005,33(8):1179-1181
建立了尿中甲基安非它明的二氯乙酰、五氟苯甲酰和3,5-二硝基苯甲酰衍生化-氮磷检测气相色谱分析方法,并与已有文献报道的乙酰、三氟乙酰、五氟丙酰、七氟丁酰等衍生化及非衍生化分析方法的灵敏度进行了比较,其中五氟苯甲酰衍生化和3,5-二硝基苯甲酰衍生化方法是比较灵敏的分析方法,尿中MA的检出限分别为3.0μg/L和4.6μg/L。  相似文献   

5.
陈捷  王志元 《色谱》2006,24(5):447-450
建立了酸水解植物蛋白及酱油中3-氯-1,2-丙二醇(3-MCPD)的固相萃取-气相色谱/质谱测定方法。样品经Aoisa-HBL固相萃取柱萃取,正己烷-乙酸乙酯净化提取,七氟丁酰咪唑衍生,衍生物经气相色谱/负化学电离-质谱(GC/NCI-MS)选择离子模式(SIM)检测,外标法定量。3-MCPD的定量检测限为0.5 μg/kg,平均回收率为92.2%~97.4%,相对标准偏差为3.6%~10.9%。该方法检测灵敏度高,定性定量准确。  相似文献   

6.
丁立平  蔡春平  王丹红 《色谱》2014,32(8):849-854
建立了同时测定蔬菜中氟吗啉和烯酰吗啉残留的改进的QuEChERS-气相色谱-质谱(GC-MS)联用法。前处理过程以乙腈高速匀浆提取样品,应用改进的QuEChERS方法对样品进行提取、盐析和净化,并采用气相色谱-质谱联用仪在选择离子监测(SIM)模式下测定了多种蔬菜中的氟吗啉和烯酰吗啉残留量,以基质匹配标准溶液外标法定量。选用DB-5 MS石英毛细管柱(30 m×0.25 mm×0.25μm),流速1.1 mL/min,采用电子轰击电离源,选择监测离子氟吗啉为m/z 285、371、165;烯酰吗啉为m/z 301、387、165。结果表明:在优化条件下,氟吗啉和烯酰吗啉在10~1000μg/kg范围内线性关系良好,相关系数不低于0.999,不同基质中的检出限(S/N=3)范围为0.67~2.42μg/kg。对于生姜、番茄、胡萝卜、菠菜、甘蓝和白木耳空白样品,在10、20、100μg/kg共3个水平下氟吗啉和烯酰吗啉的加标回收率为71%~116%,相对标准偏差(RSD)为1.8%~14.7%。同时,本研究对蔬菜中氟吗啉和烯酰吗啉残留检测的裂解机理和基质效应进行了考察。本方法具有操作简便、快速、准确的特点,可用于蔬菜中氟吗啉和烯酰吗啉残留量的日常检测。  相似文献   

7.
本文研究了苯丙胺和甲基苯丙胺的三氟乙酰、五氟丙酰、七氟丁酰、二氯乙酰、一氯二氟乙酰、五氟苯甲酰和3,5-二硝基苯甲酰的衍生化反应条件。在此基础上,建立了人尿中苯丙胺和甲基苯丙胺的酰基衍生化的气相色谱-电子捕获检测分析方法。以五氟苯甲酰衍生化法分析尿中苯丙胺的灵敏度最高,其检出限为2.0 ng/mL;采用3,5-二硝基苯甲酰衍生化分析尿中甲基苯丙胺时的灵敏度最高,检出限为5.8 ng/mL。本法简便、快速。  相似文献   

8.
建立全自动固相萃取-GC-MS/MS法检测灌溉水中乙丁烯氟灵、异丙甲草胺、乙丁氟灵、炔苯酰草胺、氟丁酰草胺5种生物高毒性除草剂残留的检测方法。将灌溉水预处理后,采用全自动固相萃取技术,选择HLB固相萃取柱对灌溉水样品进行提取。提取液经无水硫酸钠脱水后,在氮吹仪中吹至近干,1mL乙酸乙酯溶解残渣,0.22μm微孔滤膜过滤后上机气相色谱-三重四级杆质谱仪(GC-MS/MS)以多反应监测模式(MRM)扫描,外标法定量。乙丁烯氟灵、异丙甲草胺、乙丁氟灵、炔苯酰草胺、氟丁酰草胺在质量浓度0.01~0.5μg·mL-1范围内线性关系良好,定量限均为0.02μg·L-1。样品在三浓度水平的平均回收率在85.4~104.5%之间,精密度测定结果的相对标准偏差(RSD)均小于5%(n=6)。该方法自动化程度高,准确性好,为灌溉水中除草剂残留的监测提供一种分析方法。  相似文献   

9.
植物样品中痕量氟的离子色谱法分析   总被引:3,自引:0,他引:3  
建屯了碱熔法/离子色潜法测定植物样品中痕量氟的分析方法.样品于镍坩锅中500 ℃碱熔融后,经溶解、过滤,进样分析.氟离子经Metrosep A Supp 5阴离子交换柱分离,化学抑制电导检测.氟离子的线性范围为0.005~50 mg/L,相对标准偏差为5.3%,氟的检出限为0.01 mg/kg.该法适合于批量植物样品中痕量氟的测定.  相似文献   

10.
韩笑  娄喜山  张莉  王国卿  马明  王明林 《色谱》2010,28(4):341-347
建立了基质固相分散技术结合超高效液相色谱-串联质谱(UPLC-MS/MS)测定蔬菜中苯甲酰脲类杀虫剂(除虫脲、灭幼脲、杀铃脲、氟苯脲、氟虫脲、氟啶脲、氟铃脲)和双酰肼类杀虫剂(甲氧虫酰肼、虫酰肼)的方法。蔬菜样品经中性氧化铝和石墨化炭黑研磨,乙酸乙酯淋洗,洗脱液浓缩定容后,经超高效液相色谱分离,分别在正、负离子多反应监测(MRM)模式下用电喷雾电离串联质谱测定,外标法定量。结果表明,9种杀虫剂在1~100μg/L质量浓度范围内有良好的线性关系(R2≥0.99);在1、5、10、100μg/kg4个加标水平上的回收率为78.5%~112.8%;相对标准偏差为2.3%~10.2%,检出限为0.5~1.0μg/kg。该方法操作简便快速,样品和溶剂用量少,检出限低,可满足蔬菜中苯甲酰脲类和双酰肼类杀虫剂同时检测的要求。  相似文献   

11.
Electron ionization mass spectrum of sarin(Se) was interpreted in compare of sarin MS spectrum. Inhibition of butyrylcholinesterase of human plasma by sarin and sarin(Se) was determined spectrophotometrically using modified Ellman method. It appeared that after incubation with sarin and sarin(Se), cholinesterase inhibition were 93% and 83%, respectively. Sarin, sarin(Se), and sarin(Se)‐d7 were spiked into a vial containing human plasma, and albumin adduct metabolites were identified using liquid chromatography–tandem mass spectrometry. The experiments show that these agents are attached to tyrosine on albumin in human blood. Corresponding deuterated adducts were used to confirm the proposed mechanisms for the formation of the fragments in mass spectrometry experiments.  相似文献   

12.
The nerve agents are chemical warfare agents known to be used during terrorist attacks. An inexpensive and portable system to be used by first responders and military personnel is of interest owing to the continuing threat of possible terrorist attacks. Amperometric biosensors based on cholinesterase inhibition show such potentialities. In this work butyrylcholinesterase was immobilized onto screen-printed electrodes modified with Prussian blue and the nerve agent detection was performed by measuring the residual activity of enzyme. The optimized biosensor was tested with sarin and VX standard solutions, showing detection limits of 12 and 14 ppb (10% of inhibition), respectively. The enzymatic inhibition was also obtained by exposing the biosensors to sarin in gas phase. Two different concentrations of sarin gas (0.1 and 0.5 mg m−3) at different incubation times (from 30 s up to 10 min) were tested. It is possible to detect sarin at a concentration of 0.1 mg m−3 with 30-s incubation time, with a degree of inhibition of 34%, which match the legal limits (immediate danger to life and health).  相似文献   

13.
A sensitive method for the post-column reaction detection of organophosphorus compounds is described. The method relies on cholinesterase and is particularly suitable for the analysis of potent inhibitors such as sarin, soman and tabun. The compounds are separated by reversed-phase chromatography with methanol-water as the mobile phase in a linear gradient system. The reactor used for the detection comprises conventional autoanalyzer equipment with air segmentation of the reactor stream. The detection limits are 10 pg for sarin and soman and 60 pg for tabun. A quantitation method is presented, based on the linear correlation between the residual enzyme activity and the inhibitor concentration. The repeatability is +/- 1%. As a test of the system, the model compounds were detected against a background of urban air.  相似文献   

14.
Although nerve agent use is prohibited, concerns remain for human exposure to nerve agents during decommissioning, research, and warfare. Exposure can be detected through the analysis of hydrolysis products in urine as well as blood. An analytical method to detect exposure to five nerve agents, including VX, VR (Russian VX), GB (sarin), GD (soman), and GF (cyclosarin), through the analysis of the hydrolysis products, which are the primary metabolites, in serum has been developed and characterized. This method uses solid-phase extraction coupled with high-performance liquid chromatography for separation and isotopic dilution tandem mass spectrometry for detection. An uncommon buffer of ammonium fluoride was used to enhance ionization and improve sensitivity when coupled with hydrophilic interaction liquid chromatography resulting in detection limits from 0.3 to 0.5 ng/mL. The assessment of two quality control samples demonstrated high accuracy (101–105 %) and high precision (5–8 %) for the detection of these five nerve agent hydrolysis products in serum.  相似文献   

15.
Electrochemical biosensor based on electric eel acetylcholinesterase (AChE) (EC 3.1.1.7) was performed for assay of nerve agents – tabun, sarin, soman, cyclosarin, and VX. The biosensor used AChE as biorecognition element. The presence of nerve agents was accompanied by a strong inhibition of AChE activity. Enzyme activity is easily measurable by electrochemical oxidation of thiocholine created from acetylthiocholine (ATChCl) by AChE‐catalyzed hydrolysis. The tested nerve agents were successfully assayed. The best limits of detection were achieved for sarin (5.88×10?10 M) and VX (8.51×10?10 M) after one‐minute assay. The biosensor was found long term stable at low as well as laboratory temperature.  相似文献   

16.
《Analytical letters》2012,45(12):1849-1868
Acetylcholinesterase and butyrylcholinesterase are the only two known cholinesterases. Acetylcholinesterase plays an important part in cholinergic system. It terminates neurotransmission by hydrolysis of transmitter acetylcholine. The role of butyrylcholinesterase is not well understood. It is able to detoxify several compounds such as cocaine, succinylcholine, and so forth. The current review is focused on the application of cholinesterases in biorecognition. Cholinesterases are important markers in the body. Butyrylcholinesterase activity in plasma can serve as a liver function test or specific marker for sensitivity to myorelaxants or liver carcinoma. Both cholinesterases can serve as markers of poisoning by some neurotoxic compounds. Nerve agents (sarin, soman, tabun, VX), some Alzheimer disease drugs (galantamine, huperzine, donepezil, rivastigmine), pesticides (carbofuran, trichlorfon, paraoxon, malaoxon), and natural toxins (aflatoxin, pyridostigmine) can act as inhibitors of butyrylcholinesterase and/or acetylcholinesterase. Devices filled with immobilized cholinesterases can be used for the assay of the aforementioned toxins. In this review, methods for examination of cholinesterases activity in the body and in analytical devices are described. Applications, types of diagnosis, and assays are described as well.  相似文献   

17.
A rapid and simple spectrophotometric method is presented for the characterization and semiquantitative determination of toxic organophosphorus compounds. The method relies on the inhibition of various cholinesterases and involves calculation of bimolecular rate constants for reactions of compounds with cholinesterase preparations from different animal tissues. In experiments with sarin, soman, tabun, diisopropyl fluorophosphate and 2,2′-dichlorovinyldimethyl phosphate, the mean relative standard deviation obtained for the rate constants was 9%. The detection limits for the compounds were at the picogram level. The amount of compound needed for characterization, which depends on both the set of enzymes and the compound itself, was at the pg- or ng-level. As a test of the method, a concentrate of urban air spiked with sarin was examined.  相似文献   

18.
基于多层膜敏感圆片的光学式有机磷快速检测方法   总被引:1,自引:0,他引:1  
研究了基于多层膜敏感圆片的全固态有机磷光学检测方法.该方法基于胆碱酯酶抑制原理,利用紫色发光二极管光源和硅光电探测器实时测量在多层膜敏感圆片存在下待测溶液的吸光度.多层膜敏感圆片由载有胆碱酯酶和显色剂的上层亲水多孔膜片、载有底物的下层亲水多孔膜片及中间疏水性隔离膜组成.这种多层膜圆片制备简单,价格低廉,易于保存,非常适...  相似文献   

19.
For the design of a biosensor sensitive to steroidal glycoalkaloids, pH-Sensitive Field Effect Transistors as transducers and immobilised butyrylcholinesterase as a biorecognition element have been used. The total potato glycoalcaloids can be measured by this biosensor in the concentration range 0.5-100 microM with detection limits of 0.5 microM for alpha-chaconine and of 2.0 microM for alpha-solanine and solanidine, respectively. The responses of the developed biosensors were reproducible with a relative standard deviation of about 1.5% and 5% for intra- and inter-sensor responses (both cases, n=10, for an alkaloid concentration of 5 microM), respectively. Moreover, due to the reversibility of the enzyme inhibition, the same sensor chip with immobilised butyrylcholinesterase can be used several times (for at least 100 measurements) after a simple washing by a buffer solution and can be stored at 4 degrees C for at least 3 months without any significant loss of the enzymatic activity.  相似文献   

20.
《Analytical letters》2012,45(15):2521-2529
Construction of Detehit (nerve-agent detector), a colorimetric biosensor of nerve agents, enables its utilization for selective analysis of nerve agents based on the different ability of nucleophilic reagents to reactivate enzyme-inhibitor complexes in the phase before dealkylation. For this purpose mono- and bispyridinium aldoximes, common in treatment of nerve agent poisoning, are used.

For a positive identification of a pair of organophosphates, a neural network analysis was used. The analysis was processed based on spectral data of the intensity of color changes of the surface of a cotton cloth reaction zone with immobilized and stabilized enzyme acetylcholinesterase. Color changes are based on Ellman's reaction. Intensity of these changes depends on activity of the enzyme after inhibition and reactivation of enzyme-inhibitor complex. The following nerve agents were identified: sarin, soman, tabun, cyclosarin, VX, and R-33.  相似文献   

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