毛细管电泳柱上络合分离、间接紫外检测重金属离子

采用弱络合剂乙醇酸,柱上络合,间接紫外检测毛细管区带电泳(CZE)技术对重金属离子Ba2+、Cr3+、Cd2+、Pb2+及可能存在的干扰离子进行了分离研究。通过对背景电解质种类和浓度、缓冲液pH、有机添加剂等的优化,确定了最佳分离体系为含12 mmol/L络合剂乙醇酸的10 mmol/L吡啶溶液作为背景电解质(pH 4.0)。在电压15 kV,压差进样68.95 kPa.s,260 nm间接紫外检测条件下,采用50 cm(45.5 cm)×50μm(I.D.)石英毛细管,重复性实验(n=9):迁移时间RSD≤1.37%,峰高RSD≤1.70%,峰面积RSD≤3.55%;Pb2+、Ba2+和Cd3+的检出限(S/N=3)为0.2 mg/L,Cr3+的检出限为0.08 mg/L;在检出限至10 mg/L范围内,各离子的浓度与峰面积线性相关系数好于0.998。该方法并应用于实际样品的分析。     

非水体系毛细管电泳-紫外检测法测定对乙酰氨基苯酚的研究

本文报道了用非水相体系高效毛细管电泳-紫外检测法测定对乙酰氨基苯酚的新方法;考察了运行电压、非水相介质和电解质等因素的影响。在25℃下,以50mmol／L NaOH的乙醇溶液为电泳缓冲介质,30mmol／L乙酸钠的乙醇溶液为样品溶剂;选择重力进样30S,运行电压-25kV,及检测波长250nm。测定对乙酰氨基苯酚的线性范围为5．2～52μg／mL;检出限为2．88μg／mL;RSD为2．34％。本法应用于维C银翘片中对乙酰氨基苯酚的测定,结果满意。     

毛细管电泳-间接紫外法测定饮用水中草甘膦、草铵膦及其代谢产物

提出了毛细管电泳-间接紫外分析方法测定饮用水中草甘膦及其代谢产物氨甲基膦酸、草铵膦及其代谢产物3-甲基磷酸亚基丙酸。样品与25mmol·L-1乙酸铵溶液混匀后,采用SAX型固相萃取小柱提取待测物。洗脱液经毛细管电泳分离,以o-磷酸基-DL-苏氨酸为内标物,紫外检测波长为214nm。草甘膦、草铵膦、氨甲基膦酸和3-甲基磷酸亚基丙酸的线性范围为0.10~20.0mg·L-1,检出限(3S/N)分别为0.22,0.30,0.18,0.03mg·L-1,加标回收率在82.1%~108%之间。     

毛细管电泳-间接紫外法检测蜂蜜中的多种金属离子

探讨了一种利用毛细管电泳测定K+、Ba2+、Ca2+、Na+、Mg2+、Fe2+、Zn2+、Cd2+、Li+和Cu2+10种金属离子的方法。考察了紫外生色剂的浓度和pH值对分离效果的影响,并优化了分离条件。结果表明,咪唑浓度为15 mmol/L(pH 3.7),分离电压为20kV时,10种金属离子可在7min内实现基线分离。10种金属离子的线性范围为0.06～60.0mg/L,相关系数为0.9995～0.9999,检出限为0.01～0.21mg/L。标准样品的回收率为95%～104%,5次测定的相对标准偏差为0.9%～5.8%。将该法用于6个蜂蜜样品的测定,结果满意。     

毛细管电泳-间接电化学发光法对茶叶中百草枯农药残留的检测

基于农药百草枯对钌联吡啶-三丙胺(TPA)体系的电化学发光具有显著的抑制作用,建立了毛细管电泳-间接电化学发光检测茶叶中残留农药百草枯的新方法.讨论了初始电位、钌联吡啶和TPA浓度、进样电压、进样时间、运行缓冲溶液的浓度与pH值等条件对百草枯检测灵敏度的影响.确定最佳实验条件为1.20 V初始电压、0.7 mmol/L钌联吡啶、0.6 mmol/L TPA、9 kV进样电压、9 s进样时间、35 mmol/L磷酸盐(pH 8.5)为运行缓冲溶液.在优化实验条件下,百草枯浓度在5×10~(-7) 5×10~(-5)mol/L范围内呈良好线性(相关系数为0.994 5),检出限为9.4×10~(-8) mol/L.对5×10~(-5) mol/L百草枯标准溶液连续测定5次,相对峰高与迁移时间的相对标准偏差分别为3.7%和2.1%.该方法对2.0×10~(-6)、1.0×10~(-5) mol/L百草枯标样的萃取回收率分别为74%和83%,相对标准偏差分别为15%、4.2%(n=5).     

Simultaneous Determination of Inorganic Anions and Organic Acids in Environmental Samples by Capillary Zone Electrophoresis with Indirect UV Detection

Capillary zone electrophoresis (CZE) with indirect UV detection was developed for the simultaneous determination of inorganic anions and organic acids in environmental samples. Various aromatic acids (benzoic, phthalic, trimellitic, and pyromellitic acids) were evaluated as background electrolytes (BGEs) to give high resolution and detection sensitivity. Co-electroosmotic conditions such as the concentration of BGE, electrolyte pH, and EOF modifier were systematically investigated. Three inorganic anions and ten organic acids were determined simultaneously in 10 min using an electrolyte containing 10 mM phthalic acid, 0.5 mM myristyltrimethylammonium bromide (MTAB), and 5% methanol (MeOH) (v/v) at pH 5.60. Linear plots for the test solutes were obtained in the concentration range 0.01–1.0 mM with detection limits in the range 5–30 μM. The proposed method was successfully demonstrated for the determination of inorganic anions and organic acids in natural water, soil, and plant extracts after direct sample injection.     

Determination of Methamphetamine and Amphetamine by High-Performance Capillary Electrophoresis with UV Detection

Methamphetamine and amphetamine are well-known illicit drugs that have'a potent central nervous system stimulating effect. It is reported that methamphetamine is more addictive than heroin. The abuse of amphetamine and methamphetamine is increasing because they can be easily manufactured. There have been increasing interested in the development of analysis methods for methamphetamine and amphetamine. The determination of methamphetamine and amphetamine by gas chromatography (GC),GC-mass spectrometry (GC-MS), polarization fluoroimmunometry and high-performance liquid chromatography (HPLC) have been reported. Recently, Kuroda and Trenerry have reported the separation of these two compounds by CE.     

高效毛细管电泳 间接紫外吸收检测法测定食品中的氨基酸

研究了鸟氨酸、脯氨酸和谷氨酰胺的高效毛细管电泳 间接紫外吸收检测的特征。以5　mmol/L 对氨基苯磺酸钠 10 mmol/L KH2PO4(pH 11.5)为运行缓冲液,在分离电压12 kV下,于11 min实现了上述3种氨基酸的基线分离,迁移时间和峰高的相对标准偏差分别小于0.72%和2.0%,检测限分别为6.78,8.71,7.86 mg/L。应用该法测定食品中的氨基酸及各氨基酸在样品中的加标回收率,3种氨基酸的加标回收率为96.8%~104%。     

Separation of Sulfur Species in Water by Co-Electroosmotic Capillary Electrophoresis with Direct and Indirect UV Detection

Co-electroosmotic capillary electrophoresis (co-CZE) with both direct and indirect UV detection was investigated for the separation of sulfur species. With direct UV detection, the separation of S₂O^2? ₃, S₂O^2? ₄ was possible using 20 mM phosphate electrolyte containing 0.75 mM tetradecyltrimethylammonium bromide (TTAB) and 15% acetonitrile. To obtain optimal peak shape and sensitivity using indirect UV detection, a range of background electrolytes (BGEs), including benzoate, phthalate, 2,6-pyridinedicarboxylate (2,6-PDCA) and trimellitate, were examined as the BGEs. Of all the BGEs, 2,6-PDCA gave high selectivity and indirect UV response due to its mobility matching to that of sulfur species and its high absorptivity. Detection limits in range of 3-6 μM were obtained using either direct UV or indirect UV detection. The proposed CZE methods were used for the determination of sulfur species in water samples, and provided fast separation of sulfur species in less than 5 min.     

毛细管电泳-间接化学发光法分离检测儿茶酚胺及儿茶酚

根据儿茶酚胺及儿茶酚淬灭铁氰化钾-鲁米诺体系发光的原理,利用毛细管电泳．化学发光联用技术分离测定了3种儿茶酚胺和儿茶酚,并优化了检测和分离条件。在最佳条件下,测得多巴胺、肾上腺素、去甲肾上腺素和儿茶酚的检出限分别为0．33、1．8、2、4和0、12μmol／L。本方法具有一定的选择性,对于医用注射液及尿样在未经预处理条件下可直接进行分离分析,结果令人满意。     

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。     

毛细管电泳-电化学发光间接测定人血浆中盐酸甲氯芬酯

建立了一种毛细管电泳-电化学发光间接测定人血浆中盐酸甲氯芬酯(MFX)的新方法.在碱性条件下,三联吡啶钌在铂电极上的弱电化学发光信号可以被MFX增敏,且MFX水解后灵敏度比未水解的灵敏度提高了6倍.研究了工作电极电位、磷酸盐缓冲溶液浓度及其pH值、分离电压、进样电压和进样时间等实验参数对MFX水解产物N,N-二甲氨基乙醇测定的影响.在优化实验条件下,其浓度线性范围为0.020～50 μg/mL,检出限(3σ)为6.3 ng/mL,峰高的相对标准偏差为3.1%(10 μg/mL MFX,n=11).利用该法间接地测定了人血浆中MFX的含量,回收率为95.9%～96.9%.     

Determination of Anionic Surfactant Turkey Red Oil by Capillary Electrophoresis with Direct UV Detection

A method using capillary electrophoresis with direct UV detection has been developed and validated for the determination of Turkey Red Oil (sulfonated castor oil). The highest performance with respect to separation efficiency and analysis time was achieved with 30 mM Tris (pH 8.0) buffer containing 7.5 mM HP-β-CD. The feasibility of the proposed CE method for the analysis of Turkey Red Oil surfactant in industrial water samples is demonstrated. Spiking of real samples gave recoveries between 90 and 106%. The CE results were compared with that obtained by GC-MS. It was concluded that CE can be a good alternative for fast determination of Turkey Red Oil component distribution in industrial process waters with no sample preparation other than dilution. However, the method sensitivity is not satisfactory for monitoring surfactant level in a waste effluent stream.     

毛细管电泳-间接紫外检测法分离和测定食品中的有机酸

有机酸毛细管电泳（CE）分析是90年代初首先被报道的[1],近年来有了较大的发展[2]．采用CE法可进行不同基质样品如食品、饮料、尿液等样品中多种有机酸的同时分析[1,3,4]．该法采用CE的阴离子分离模式,在电解质溶液中加入电渗流改性剂,使电渗流方向逆向,从而与阴离子的电泳方向一致,以缩短分析时间．常见有机酸在200um以上大多无紫外吸收,一般采用间接紫外检测方法[1,3],也可采用低波长紫外检测[4]．低分子量阴离子的CE研究报道不多[5,6],有机酸的CE分离系统研究尚未见报道．本文系统地研究了毛细管电泳-间接紫外检测法分析…     

非水毛细管电泳/紫外检测法测定肉桂中的肉桂酸和肉桂醛

建立了用非水相体系高效毛细管电泳/紫外检测法同时测定肉桂酸和肉桂醛的新方法,考察了运行电压、非水相介质和电解质等因素的影响。在25℃下,以乙腈和碳酸丙烯酯(体积比3∶2)的混合液为缓冲体系的溶剂,缓冲体系中含25 mmol/L十六烷基三甲基溴化铵,0.375%(φ)乙酸,以碳酸丙烯酯为样品溶剂,重力进样30 s,运行电压20 kV,毛细管总长45 cm,有效长度30 cm,φ75μm,检测波长310 nm。肉桂酸线性范围为4~100 mg/L,r=0.999 4,检出限为0.80 mg/L,RSD为1.07%。肉桂醛的线性范围10~240 mg/L,r=0.999 6,检出限为2.30 mg/L,RSD为2.19%。应用于肉桂中的肉桂醛和肉桂酸的测定,结果满意。     

毛细管电泳-间接激光光热干涉检测方法研究

本文提出毛细管电泳-间接激光光热干涉检测新方法。采用吸收系数大、吸收波长与泵浦激光(He-Ne)波长匹配性能较好的亚甲蓝溶液为背景电解质溶液,加入乙醇减少了毛细管壁对亚甲蓝的吸附作用。并将间接光热干涉检测法用于氨基酸毛细管电泳分离检测,对赖氨酸检测限达5×10^-6mol/L(S/N=2).     

茶叶中无机阴离子的毛细管电泳分离间接检测方法的研究

建立了毛细管电泳分离测定茶叶中Cl-、NO2-、NO3-、SO42-、F-及HPO24-的方法。通过研究分离电压、背景电解质和电渗流改性剂的浓度、pH的影响优化了分析条件。在优化条件下,6种无机阴离子在10min内得到完全分离,各组分迁移时间和峰高的相对标准偏差(RSD)分别为1.9%~4.7%和1.2%~3.8%,检出限为0.11~0.82 mg/L。通过分析实际样品并做加标回收实验验证了该方法的可行性,Cl-、NO3-、SO42-及HPO24-的回收率为93%~98%。     

毛细管电泳电化学检测单糖的研究

采用毛细管区带电泳直立式安培电化学检测方法分离和测定单糖。考察了电解质溶液的ＰＨ和浓度对单糖分离的影响，适量加入氯化钠可改善分离条件。应用该法进行了乳糖的组成和人血中葡萄糖的测定。     

喜树果中喜树碱含量的高效毛细管电泳安培法测定

建立了喜树果中喜树碱的高效毛细管电泳安培检测方法.着重探讨了缓冲溶液种类、浓度、酸碱度及操作电压、进样时间等对检测的影响.Na2B4O7-NaOH(Na2B4O7浓度为30 mmol/L)为电泳介质,在15 kV高压,pH 9.0的碱性条件下用柱端安培检测喜树碱含量.该法的线性范围为:1～100 mg/L,Y=11 020 1 014.6 ρ,r=0.999 4,检出限为0.5 mg/L.