毛细管电泳用β-环糊精作改性剂分离血清中吗啡和可待因

建立了血清中吗啡和可待因的毛细管电泳分离分析方法。讨论了电泳分离模式、缓冲液pH,β-环糊精（β-CD）浓度对分离的影响。吗啡和可待因检测限均为0．1μg/mL，不同浓度的萃取回收率分别大于92％和93％，迁移时间的相对标准偏差分别小于0．44％和0．39％，峰面积的相对标准偏差分别小于3．2％和4．1％。     

吗啡和海洛因等生物碱的高效液相色谱化学发光测定

研究了吗啡、可待因、Ｏ＾３单乙酰吗啡和海洛因等生物碱在多聚磷酸介质中与高锰酸钾的发光行为和光谱现象。建立了反相 高效液相色谱化学发光检测吸毒者尿液和雅片中吗啡、可待因等物质的方法。     

毛细管电泳-间接化学发光法检测尿液与血液中吗啡含量

在碱性溶液中,吗啡对Ag(Ⅲ)配合物-鲁米诺化学发光体系的化学发光信号有显著抑制作用,且抑制程度与吗啡浓度成正比。基于此,建立了毛细管电泳-间接化学发光检测尿液和血液中吗啡含量的方法。在优化条件下,方法检出限为0.75 mg/L,线性范围为2.0~30.0 mg/L,相关系数(r)为0.999 8;对20mg/L的吗啡进行7次平行测定,测得的相对标准偏差(RSD)为2.0%。结合固相萃取法,该方法成功用于尿液和血液中吗啡含量的测定,平均加标回收率分别为109.0%与101.3%。该方法分辨率高、灵敏、分析成本低,可用于尿液和血液中吗啡含量的测定。     

头发中单乙酰吗啡和吗啡检测的研究

建立了用ＧＣ－ＭＳ技术检测人头发中毒品海洛因的主要代谢产物６－单乙酰吗啡和吗啡的方法。以乙基吗啡为内标，样品酸水解后用混合有机溶剂提取。提取物经Ｎ－甲基－Ｎ－三甲基硅基三氟乙酰胺（ＭＳＴＦＡ）衍生化，采用ＧＣ－ＭＳ定性定量分析。该法已用于确认经常性滥用海洛因的实际检案分析     

液相色谱化学发光检测法的新进展

本文评述了近年来液相色谱化学发光检测法的新进展，内容涉及各类化学发光发反应，生物发光反应和电致化学发光反应同色谱体系的偶合方式，仪器设计，多种无机，有机，生物大分子和生物活性物质的分析方法及其在环境，生物医学科学和生命科学中的应用和发展方向。引用文献１６８篇。     

添加剂对十二烷基磺酸钠溶液性质影响的研究

添加剂对十二烷基磺酸钠溶液性质影响的研究＊鲁润华郝京诚汪汉卿（中国科学院兰州化学物理研究所兰州７３００００）关键词表面张力电导添加剂Ａｓ中图分类号Ｏ５５２．４添加剂对表面活性剂溶液物理化学性质影响的研究是人们极感兴趣的研究内容［１］，因为表面活性剂实...     

硅胶负载β—环糊精催化剂用于4—羟基苯甲酸的选择性合成

制备了一种新的硅胶负载β－环糊精催化剂，考察了其对苯酚的催化羧化作用。实验结果表明，硅胶 负载β－环糊精对苯酚对位羧化的位选择性近１００％。     

化学发光免疫技术

化学发光免疫技术是化学发光与免疫测定结合起来的一种高效检测手段,化学发光是在特定化学反应中产生的光辐射。化学发光免疫技术可根据抗原抗体标记物的不同而分为发光物免疫测定、发光酶免疫测定和发光辅助因子免疫测定三大类型。     

β—CD对Zn（Ⅱ）—m—BrTPPS4显色反应增敏作用的研究

本系统研究了β－ＣＤ对Ｚｎ（Ⅱ）－ｍ－ＢｒＴＰＰＳ４显色体系的增敏作用，提出了高灵敏度测定痕量锌的分光光度新方法。显色体系的表观摩尔吸光系数为４．５７×１０＾５Ｌ．ｍｏｌ＾－＾１．ｃｍ＾－＆１，Ｚｎ（Ⅱ）的浓度在０－５μ／２５ｍＬ符合比定律。应用本法于发，铝合金等试样中锌的测定，回收率及方法对照结果令人满意。     

基于核酸适配体的化学发光检测腺苷

以羧基磁性微球为分离载体,固定氨基修饰的腺苷适配体,通过腺苷与生物素修饰的报告序列竞争结合氨基适配体,建立了一种化学发光检测生物小分子腺苷的方法。实验优化了磁性微球、氨基适配体、报告序列等参数,发现腺苷浓度在1.0×10-9~1.0×10-4 mol/L范围内与CL信号强度减少量呈良好线性关系,最低检出限达1.0×10-9mol/L,重复5次测定0.1 mmol/L腺苷的相对标准偏差为5.0%。方法成功用于实际尿样中腺苷的测定。该法可简单、灵敏、特异性地检测腺苷,有望用于临床诊断、药物分析等领域。     

Chemiluminescent Detection of Gatifloxacin Residue in Milk

Abstract

An indirect competitive chemiluminescent enzyme-linked immunosorbent assay (CL-ELISA) for detection of gatifloxacin residue in milk was developed in this study. Compared with conventional colorimetric ELISA using the same antibody, the developed CL immunoassay shows a significant improvement in sensitivity and detectability with an IC₅₀ of 0.4 ng mL^?1 and a detection limit of 0.001 ng mL^?1 and thus is suitable to be used as a highly sensitive screening method to detect and regulate illegal use of gatifloxacin in food and food products. The test kit was applied to detect milk samples spiked by gatifloxacin, and satisfactory results were obtained.     

流动注射化学发光增强法测定单宁酸

发现单宁酸对Luminol KIO4 Mn2 +碱性体系的化学发光有较强增敏作用 ,据此建立了流动注射化学发光增强法测定单宁酸的新方法。该法简单、快速、线性范围宽 ,测定单宁酸的检出限为 9× 10 -9mol/L ;线性范围为 3× 10 -8～ 5× 10 -6mol/L ,对于 1× 10 -6mol/L单宁酸测定的相对标准偏差 1 5 % (n =11)。应用于五倍子中单宁酸的测定 ,结果满意。     

Chemiluminescent Detection of Carbohydrates in the Tumoral Breast Diseases

Nowadays, there is an increase of investigations into the fibroadenoma, mainly because some studies have shown that the occurrence of fibroadenoma is linked to an increased risk of developing breast carcinoma. Currently, the chemiluminescence biomarkers are applied for validation methods and screening. Here, a lectin chemiluminescence is proposed as new histochemistry method to identify carbohydrates in mammary tumoral tissues. The lectins concanavalin A (Con A) and peanut agglutinin (PNA) conjugated to acridinium ester were used to characterize the glycocode of breast tissues: normal, fibroadenoma, and invasive duct carcinoma (IDC). The lectin chemiluminescence expressed in relative light units (RLU) was higher in fibroadenoma and IDC than in normal tissue for both lectins tested. The relationship RLU emission versus tissue area described a linear and hyperbolic curve for IDC and fibroadenoma, respectively, using Con A whereas hyperbolic curves for both transformed tissues using PNA. RLU was abolished by inhibiting the interaction between tissues and lectins using their specific carbohydrates: methyl-α-d-mannoside (Con A) and galactose (PNA). The intrinsic fluorescence emission did not change with combination of the lectins (Con A/PNA) to the acridinium ester for hydrophobic residues. These results represent the lectin chemiluminescence as an alternative of histochemistry method for tumoral diagnosis in the breast.     

化学发光色谱柱后检测技术及其应用

化学发光(chemiluminescence,CL)检测的最大特点是设备简单、分析速度快及灵敏度高,是一种有效的微量和痕量分析手段,已在环境科学、临床检验、药学、工业分析等领域得到广泛的应用[1～3]。但是,化学发光分析法也存在着选择性差的问题,从而限制了这一方法的应用范围。高灵敏度的CL检测手段与高分辨的高效液相色谱(HPLC)、毛细管电泳(CE)和微流控芯片等分离技术相结合,成为一种理想的分离分析方法,得到人们的广泛重视。20世纪80年代的毛细管电泳和90年代初微流控芯片的出现、分析仪器的微型化和进样量少的要求向科研人员提出了要解决…     

苯二酚异构体的高效液相色谱化学发光检测法研究

高效液相色谱作为一种有效的分离手段已被用于酚类化合物的分析 ,紫外检测法 [1～ 3] 、电化学检测法[3,4 ] 等已用于苯二酚异构体的测定 ,但苯二酚异构体的化学发光检测法尚未见文献报道 .前文 [5] 结果表明 ,苯二酚异构体等对鲁米诺诱导的化学发光具有很强的抑制作用 .基于此 ,本文将高效液相色谱与化学发光技术联用 ,首次建立了苯二酚异构体的高效液相色谱化学发光检测法 .该法灵敏度高 ,选择性好 ,为酚类物质的测定提供了一条新的途径 .1　实验部分1 .1　仪器与试剂　 FIA- 2 4 0 0型流动注射分析仪 (中国科学院信通科学仪器公司 ) ;G…     

Near-Infrared Photodynamic Chemiluminescent Probes for Cancer Therapy and Metastasis Detection

There is growing interest in the development of chemiluminescence (CL) probes for phototheranostics because of their minimized tissue autofluorescence. However, due to a lack of near-infrared (NIR)-absorbing chemiluminophores, current probes for NIR CL-guided phototherapy are based on nanoparticles made up of multiple components. We report bright unimolecular chemiluminophores with NIR absorptions and emissions, long CL half-lives and ideal photodynamic efficiency. One luminophore is modified into an activatable probe, DBP_OL, with a turn-on CL signal and photodynamic activity that are specific to a cancer biomarker. The highly sensitive DBP_OL allows CL-guided photodynamic therapy which completely inhibits tumor growth and lung metastasis in mouse models, and can be applied for noninvasive monitoring of lung metastasis. We provide molecular guidelines for NIR-absorbing CL probes for imaging-guided phototherapy.     

Persistent Chemiluminescent Glow of Phenoxy-dioxetane Luminophore Enables Unique CRET-Based Detection of Proteases

Chemiluminescence is being considered an effective imaging modality as it offers low background and high sensitivity. Recent discovery by our group has led to development of new phenoxy-dioxetane chemiluminescence luminophores, which are highly bright under physiological conditions. However, the current scope of probes based on these luminophores is limited, as they can only be turned on by phenol protecting group removal. Here we present a new chemiluminescence resonance energy transfer (CRET) system, Glow-CRET, in which light emission is triggered by proteolytic cleavage of a peptide substrate that links a dioxetane luminophore and a quencher. In order to compose such system, a new phenoxy-dioxetane luminophore, 7-HC-CL, was developed. This luminophore exhibits intense and persistent glow chemiluminescence; it undergoes very slow chemiexcitation, and it has the highest chemiluminescence quantum yield ever reported under physiological conditions. Based on 7-HC-CL, a Glow-CRET probe for matrix metalloproteinases, MMP-CL, was synthesized. Incubation of MMP-CL with its cognate protease resulted in 160-fold increase in chemiluminescence signal. MMP-CL was also able to detect matrix metalloproteinase activity in cancer cells with significantly higher signal-to-background ratio than an analogous fluorescence resonance energy transfer (FRET)-based probe. This work is expected to open new horizons in chemiluminescence imaging, as it enables to use the dioxetanes in ways that had not been possible. We anticipate that 7-HC-CL and future derivatives will be utilized not only for the construction of further Glow-CRET probes, but also for other applications, such as chemiluminescence tagging of proteins.     

Chemiluminescent Detection of HIV DNA Based on Allosteric Activation of Peroxidase-Mimicking DNAzyme

Homogeneous chemiluminescent method for HIV DNA detection based on allosteric activation of peroxidase-mimicking DNAzyme (PMDNAzyme) was developed. The probes used in the assay contain PMDNAzyme fragment and the additional oligonucleotide sequence complementary to HIV DNA. The interaction of PMDNAzyme fragment and the additional oligonucleotide sequence results in changes in G-quadruplex structure of the PMDNAzyme and decreases peroxidase-like activity of the probe. In the presence of HIV DNA such interaction was destroyed due to the formation of stable duplex between the additional fragment of the probe and DNA-analyte. Consequently, some reorganizations in G-quadruplex structure of the probe are observed, which are accompanied by enhancement of catalytic activity of the PMDNAzyme. The mechanism of the DNA-dependent activation of PMDNAzyme containing probes was confirmed by CD spectroscopy as well as modeling of the probes and their complexes with DNA target. The calibration curves for HIV DNA determination allowed estimating the analytical parameters of the assay. The detection limit value and the linear range were shown to be 0.3 nM and 0.3–15 nM, respectively. The assay sensitivity was high (190000 nM^–1). The values of coefficient of variation (CV) measured within the working range varied less than 4%, which indicates the high accuracy of the proposed assay.