共查询到20条相似文献,搜索用时 15 毫秒
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MinHAO DaXING QunCHEN JuanWANG 《中国化学快报》2004,15(6):679-682
This paper, for the first time, reports a method that can be used as a highly sensitive probe for singlet oxygen (^1O2) and superoxide anion (O2^-) in vitro or in vivo. FCLA(3,7-dihydro-6-{4-[2-(N‘-(5-fluoresceinyl)thioureido)ethoxy]phenyl}-2-methylimidazo{1,2-a}pyrazin-3-one sodium salt), a chemiluminescence (CL) analysis reagent, has been reported to sensitively react with ^1O2 and O2^- to emit photons with a spectral peak of 525nm. In this work,when human serum albumin (HSA) was added into FCLA solution to enhance the CL intensity,approximately 20 times, compared to that without HSA. The enhanced CL had the same 525 nm spectral peak, identical to that without HSA. By gradually reducing the molecular oxygen content in the solution, we find that the auto-oxidation of oxygen molecules dissolved in the solution plays an important role in the CL process. Based on these experimental evidences, we propose a novel and highly sensitive detection method of ^1O2 and O2^- which may have a great potential in chemical and medical applications. 相似文献
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Ewa Jaszczak-Wilke Krystyna Kozio Bogumia Kiebratowska aneta Polkowska 《Molecules (Basel, Switzerland)》2021,26(15)
The parents’ addictions and eating habits have a significant influence on the child’s growth. The first stool of a newborn baby provides a large amount of information about xenobiotics transmitted by the mother’s body. The analytical technique used in the study is ion chromatography with pulsed amperometric detection (IC-PAD). The biological samples, which were obtained from women staying in a maternity ward and their partners, revealed cyanide concentrations in urine samples spanning 1.30–25.3 μg L−1. Meanwhile, the results of the meconium samples were in the range of 1.54 μg L−1 to 24.9 μg L−1. Under the optimized chromatographic conditions, the IC-PAD system exhibited satisfactory repeatability (R < 3%, n = 3) and good linearity in the range of 1–100 μg L−1. Thus, it proved to be an effective tool for monitoring trace cyanide concentration in a series of human body fluid matrices, including meconium. Based on the literature review, this is the first application of the IC-PAD analytical technique for the determination of cyanide ions in meconium samples. 相似文献
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建立离子色谱安培法检测尿液中胱氨酸的分析方法。将尿液稀释处理后,过OnGuardⅡRP前处理柱,去除尿液中的有机物,选用低容量阳离子交换柱IonPac CS17进行分离,以甲烷磺酸梯度淋洗,柱后用300 mmol/L NaOH溶液衍生,离子色谱脉冲安培法检测,外标法定量。胱氨酸的质量浓度在0.1~5.0 mg/L范围内与其色谱峰面积呈良好的线性,线性相关系数r^2=0.999 9,检出限为0.05 mg/L。测定结果的相对标准偏差为0.71%(n=6),样品加标回收率为94%~108%。该方法具有操作简单,专属性强,灵敏度高等优点,可用于临床快速检测尿液中的胱氨酸。 相似文献
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中毒患者血清和尿液中毒鼠强残留物的GC-MS分析方法 总被引:2,自引:0,他引:2
有关资料表明,人和动物口服毒鼠强后,其血液、尿液和各脏器中均有毒鼠强残留物出现,残留时间从药后数小时至几天乃至十几天之内不等。可见血液和尿液作为可印证中毒病人中毒原因的直接样品更值得我们去关注,与呕吐物、可疑食物等检品相比,它具有提取相对简单,干扰成分少,残留时间长以及可反复采集等许多优点。因此,我们结合突发性中毒检验工作的需要,利用超声波液-液萃取技术,研究了中毒患者血清和尿液中毒鼠强残留物的GC-MS-SIM检测方法。在对40多人份血清和尿液添加标准物的反复测定中,回收率血清保持在90.8%~99.5%;RSD为3.82%,尿液保持在91.2%~102.8%,RSD为4.91%,全过程仅需约30min。经过两年来百多份样品检测的验证,该方法不失为日常快速分析中毒患者血清和尿液中毒鼠强残留物的一种有效方法,现介绍如下。 相似文献
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Mädler S Barylyuk K Boeri Erba E Nieckarz RJ Zenobi R 《Journal of the American Society for Mass Spectrometry》2012,23(2):213-224
Chemical cross-linking in combination with high-mass MALDI mass spectrometry allows for the rapid identification of interactions
and determination of the complex stoichiometry of noncovalent protein–protein interactions. As the molecular weight of these
complexes increases, the fraction of multiply charged species typically increases. In the case of homomeric complexes, signals
from multiply charged multimers overlap with singly charged subunits. Remarkably, spectra recorded in negative ion mode show
lower abundances of multiply charged species, lower background, higher reproducibility, and, thus, overall cleaner spectra
compared with positive ion mode spectra. In this work, a dedicated high-mass detector was applied for measuring high-mass
proteins (up to 200 kDa) by negative ion mode MALDI-MS. The influences of sample preparation and instrumental parameters were
carefully investigated. Relative signal integrals of multiply charged anions were relatively independent of any of the examined
parameters and could thus be approximated easily for the spectra of cross-linked complexes. For example, the fraction of doubly
charged anions signals overlapping with the signals of singly charged subunits could be more precisely estimated than in positive
ion mode. Sinapinic acid was found to be an excellent matrix for the analysis of proteins and cross-linked protein complexes
in both ion modes. Our results suggest that negative ion mode data of chemically cross-linked protein complexes are complementary
to positive ion mode data and can in some cases represent the solution phase situation better than positive ion mode. 相似文献
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基于离子迁移谱的爆炸物探测仪多采用放射性电离源,发展非放射性电离源一直是该技术的研究热点。本研究基于电晕放电原理设计了一种新型负电晕放电电离源结构,结合自行研制的离子迁移谱仪,应用于痕量爆炸物的快速、高灵敏检测。单向气流模式下,对此电离源的气流、放电电压等运行参数进行了系统优化,得到最佳实验条件为:电晕放电电离源结构的电极环孔直径为3 mm,针-环距离为2 mm,放电电压为2400 V,漂气流速为1200 mL/min。在此条件下,避免了放电副产物氮氧化物和臭氧等引发的一系列复杂反应,得到了单一的反应试剂离子O-2(H2O)n。将其应用于爆炸物,如2,4,6-三硝基甲苯(TNT)、硝酸铵(AN)、硝化甘油( NG)、太安( PETN)、黑索金( RDX)等的高灵敏快速直接检测,对TNT的检测限达到200 pg/μL。结果表明,此负电晕放电电离源具有灵敏度高、结构简单、无辐射性、反应试剂离子单一等优点,在爆炸物快速高灵敏检测、公共安全保障等方面具有广阔的应用前景。 相似文献
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柱前荧光衍生-高效液相色谱法测定尿和血清中的环境雌激素 总被引:8,自引:0,他引:8
建立了同时测定人尿和血清中环境雌激素双酚A、4-壬基酚、17α-乙炔基雌二醇及内源性雌激素雌三醇、17α-雌二醇和17β-雌二醇的对硝基苯甲酰氯柱前荧光衍生-高效液相色谱测定方法。尿样经酸水解、固相萃取柱浓缩、净化分离;血清样品经乙腈沉淀蛋白后,用乙醚萃取游离态雌激素,N2气流挥干、在无水条件下,雌激素与对硝基苯甲酰氯反应生成荧光产物,用高效液相色谱法定量。检出限为2.7—8.3μg/L;加标回收率尿样为78.0%-102.5%,血清样为72.6%-98.6%;方法精密度为1.29%-4.52%。应用本法对20份尿样和10份血清样进行了测定,结果满意。 相似文献
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提出了气相色谱-质谱法测定水中雌二醇、雌酮、雌三醇、戊酸雌二醇、己烯雌酚、乙炔雌二醇、双酚A和壬基酚等8种雌激素含量的方法。样品经乙酸乙酯提取和HLB小柱净化后,所得净化液中的雌激素与三甲基硅基化剂(TMS)或七氟丁酸酐(HFBA)进行衍生化反应产物用正己烷定容。在气相色谱分离中用DB-5MS毛细管柱为固定相,在质谱分析中采用全扫描和选择离子监测模式。8种雌激素的峰面积与质量浓度在20.0~1 000μg.L-1范围内呈线性关系,检出限(3S/N)在0.1~0.5μg.L-1之间。方法用于水中雌激素的测定,回收率在71%~103%之间,相对标准偏差(n=6)在4.2%~15%之间。 相似文献
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氯氮平,化学名称为8-氯-11-(4-甲基-1-嗪基)-5H-二苯并[b,e][1,4]二氮杂革(C18H19CIN4,Mr=326.81).纯品为淡黄色结晶性粉末,从丙酮或石油醚中得到黄色结晶,MP183~184℃,易溶于氯仿,溶于乙醇,略溶于异丙醇,几乎不溶于水. 相似文献
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Qi Wan Ling Han Yunchuan Guo Huijun Yu Li Tan Ai Zheng Yali Chen 《Molecules (Basel, Switzerland)》2021,26(23)
Ovarian cancer has the highest mortality rate in the world. Therefore, it is urgent but still challenging to develop an efficient circulating tumor cell (CTC) detection method to sensitively detect ovarian cancer. To address such issues, herein, for the first time, we present a novel CTC detection method for ovarian cancer cells by designing sensitive and rapid graphene-based biosensors. This graphene-based sensor, consisting of a cell pool and two electrodes, can be prepared by a conventional chip fabrication process. It demonstrates high-sensitivity detection even for several ovarian cancer cells by comparing the electrical signal before and after adding cell solution. Moreover, the graphene-based biosensors can perform rapid detection with good repeatability. This suggests that this novel method is possible to use for the early detection of ovarian cancer with very low CTC cell concentration. This work provides a novel and quick strategy to detect ovarian cancer and further judge or predict the risk of the transfer of ovarian cancer. 相似文献
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气相色谱-质谱法测定尿及河底泥中的环境雌激素 总被引:38,自引:3,他引:38
报道了尿及河底泥中环境雌激素(壬基酚、双酚A、己烯雌酚、17α-乙炔基雌二醇)和内源性雌激素(17α-雌二醇、17β-雌二醇、雌三醇、雌酮)的气相色谱-质谱(GC-MS)测定法。尿样经盐酸溶液水解后用固相萃取(SPE)柱浓缩净化,底泥样品用甲醇-乙酸乙酯萃取。被测组分经五氟丙酸酐(PFPA)衍生化后用GC-MS进行定性定量检测。该法测定的峰面积的日内相对标准偏差为1.22%-5.55%,检出限为0.05-1.27 μg/L(或μg/kg)。被测组分的加标回收率除尿样中17α-乙炔基雌二醇和己烯雌酚分别为2 相似文献
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DNA电泳芯片快速检测系统的设计与实现 总被引:7,自引:0,他引:7
引 言近年来 ,出现了基于微电子机械技术 (MEMS)的电泳芯片技术 ,已经被应用于蛋白质等生物大分子的分离分析、DNA测序、药物分析等领域。由于芯片中分析的样品量仅有几十皮升 ,电泳时间的缩短至几分钟 ,必须采用高灵敏度、快速的检测方法。本文提出了一种激光激发的荧光快速检测方法。检测限已达到 1 0 -19mol。2 系统设计2 .1 仪器与设备 367型 1 0mW氩离子激光器 (南京电子管厂 ) ;半反半透镜 ( 50 5DRLP ,545DRLP ,570DRLP ,590DRLP ,OmegaOptical公司 ) ;单色滤光片 ( 52 5DF30 ,5… 相似文献
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GC法测定青岛某水体中雌激素含量 总被引:10,自引:0,他引:10
介绍了测定环境水中几种雌激素,如:雌酮(E1)、雌二醇(E2)、雌三醇(E3)和雌炔醇(EE2)的测定方法.用C-18小柱对水体中的雌激素进行富集.研究了用TFA、MSTFA对雌激素的衍生化条件.GC-FID及GC-MS法测定衍生化雌激素的工作曲线,相关系数在0.98~0.99之间.测得500 mL实际水样中的加标回收率为86%~120%.5 000 mL环境水样的方法检测限为1~3 ng/L.用GC-MS法测定了海水和河水中的雌激素含量. 相似文献
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人尿中克仑特罗的测定 总被引:8,自引:0,他引:8
本文采用直接液-液萃取和TMS衍生化方法,利用GC/MS选择离子检测技术对人尿中的克仑特罗进行了分析研究,建立了灵敏的分析方法。给出了克仑特罗的回收率、检测限及人尿中的排泄曲线。 相似文献