基于高灵敏探针海萤荧光素类似物的化学发光法检测尿微量白蛋白

海萤荧光素类似物FCLA能检测1O2并产生532nm的化学发光,白蛋白(HSA)能强烈增强FCLA-1O2化学发光。基于此,建立了一种有效、高灵敏的检测HSA的化学发光(CL)检测技术。在选定的最佳实验条件下,HSA浓度与增强化学发光信号在0.34～5.5mg/L之间呈良好的线性关系;检出限为0.017mg/L(3σ)。对比荧光光谱分析法、同步荧光扫描法及瑞利光散射法等传统方法,本方法成本低廉、灵敏度高。实际尿样检测与临床检测结果一致,同时还初步探讨了HSA增敏CL的机制。     

流动注射化学发光法测定尿酸

在碱性条件下,铁氰化钾氧化鲁米诺,产生化学发光,尿酸对该体系的化学发光有显著的增强作用（亚铁氰化钾存在时）。基于此,建立了一种直接测定尿酸的流动注射化学发光分析法。方法的线性范围为２．０×１０－８～５．０×１０－６　ｇ／ｍＬ;检测限（３σ）为６．７×１０－９　ｇ／ｍＬ;相对标准偏差为１．１％（尿酸１．０×１０－７　ｇ／ｍＬ,ｎ＝１１）。用于血清及尿样中尿酸的分析,结果令人满意。     

流动注射化学发光法测定没食子酸

基于在碱性介质中,没食子酸(Gallicacid)被过氧化氢氧化能产生化学发光,而甲醛对该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法测定没食子酸的新方法。该法简单、快速、线性范围较宽。本法测定没食子酸的线性范围为2.0×10-6～2.0×10-4g/mL,检出限达5.8×10-7g/mL,采样频率为120个/小时。对4.0×10-5g/mL没食子酸溶液连续11次测定的相对标准偏差为2.52%。该方法已成功地用于橄榄中没食子酸含量的测定。     

Application of Lanthanide-Sensitised Chemiluminescence to the Determination of Levofloxacin, Moxifloxacin and Trovafloxacin in Tablets

A flow injection method including chemiluminescence detection has been developed and applied to the determination of fluoroquinolones levofloxacin, moxifloxacin and trovafloxacin in tablets. The proposed method is based on the luminescent properties of the system Ce(IV)–sulphite–fluoroquinolone and the addition of a trivalent lanthanide ion as emission-sensitizer. The optimum conditions for chemiluminescence emission were investigated for each fluoroquinolone. The best results were achieved when employing Eu(III) as lanthanide cation for levofloxacin and moxifloxacin, and Tb(III) for trovafloxacin. These fluoroquinolones were determined over the concentration range of 0.5–3.5µgmL^–1, 0.2–3.0µgmL^–1 and 0.008–0.400µgmL^–1, with detection limits of 0.100, 0.035 and 0.008µgmL^–1, respectively. The relative standard deviations were in the range of 1.0–2.5% for all three cases. The method was applied to the determination of three fluoroquinolones in their respective pharmaceutical preparations and compared with an independent UV-spectrophotometric method. The results were satisfactory.     

高灵敏反相流动注射化学发光法测定抗坏血酸

基于抗坏血酸对Ｆｅ２＋－Ｌｕｍｉｎｏｌ－Ｏ２体系化学发光的抑制效应，利用反相流动注射技术，建立了一个测定抗坏血酸的高灵敏化学发光新方法。该法检出限达２×１０－１０ｇ／ｍＬ；抗坏血酸浓度在 １×１０－９～１× １０－６ｇ／ｍＬ范围内与体系化学发光强度减小量呈良好线性相关；相对标准偏差为１．９％（Ｃ＝５×１０－８ｇ／ｍＬ，ｎ＝１１）。     

流动注射化学发光法测定叶酸

建立了用高锰酸钾 -硫酸 -甲醛 -叶酸化学发光体系测定叶酸的新方法。方法的检出限为 2 .4× 10 -8mol/ L,叶酸浓度在 1.0× 10 -7～ 1.0× 10 -5 mol/ L范围内与化学发光强度呈良好的线性关系。对 4.0× 10 -6 mol/ L叶酸进行 11次平行测定 ,方法的相对标准偏差为 1.7%。该法用于叶酸片剂中叶酸含量的测定 ,结果与药典标准方法测得值一致 ,回收率为 97.3%～ 10 3.8%。     

Flow Injection Chemiluminescence Determination of Phenol in Neutral Medium

A new flow injection chemiluminescence method for the determination of phenol was proposed, based upon the chemiluminescence reaction of phenol, N-bromosuccinimide, and hydrogen peroxide in neutral aqueous medium in the presence of cetyltrimethylammonium bromide surfactant micelles. The chemiluminescence signal was proportional to the concentration of phenol in the range of 1.0 × 10^?7?8.0 × 10^?6 g/mL with a detection limit of 3 × 10^?8 g/mL. The relative standard deviation for 1.0 × 10^?6 g/mL phenol solution was 2.0% (n = 11). The proposed method was successfully applied to the determination of phenol in phenol ear drops. A possible CL reaction mechanism was also discussed briefly.     

检测DL-苹果酸的高锰酸钾化学发光体系

利用高锰酸钾化学发光体系测定了DL-苹果酸 ,测得该物质的浓度与其对应的化学发光峰值在一定范围内存在较好的线性关系。测定DL-苹果酸的线性范围在1.0×10-6～1.0×10-2mol·L-1;相对标准偏差为1.4%(n=8) ,检出限为1.0×10-9mol·L-1。测定实际苹果汁与饮料 ,结果良好。实验表明 ,该法线性范围宽、重现性好、操作简便。文中还探讨了该体系的自催化属性。     

反相流动注射化学发光法测定单宁

在碱性介质中 ,单宁对高碘酸钾氧化鲁米诺的化学发光反应有较强的增敏作用 ,据此建立了反相流动注射化学发光测定单宁的新方法 ,并研究了最佳反应条件。该方法快速、准确、线性范围宽 ,测定单宁的检出限为 1 .1 2× 1 0 - 9g/ m L,方法的线性范围为 2 .0× 1 0 - 8～ 6 .0× 1 0 - 6 g/ m L,对于 4.0× 1 0 - 6 g/ m L单宁 1 0次测定的相对标准偏差为 0 .79%。应用于中药五倍子、诃子中单宁的测定 ,结果满意     

鲁米诺-高碘酸钾-抗坏血酸体系化学发光反应的研究与应用

基于抗坏血酸在碱性条件下与高磺酸钾和鲁米诺反应产有强的化学发光,建立了流动注射化学发光测定抗坏血酸的新方法。在碱性条件下的氧化过程易产生过氧化物和超氧自由基,是产生化学发光的关键。该法校准曲线线性范围为６．０×１０＾－６－４．０×１０＾－２ｇ／Ｌ,检出限达８×１０＾－７ｇ／Ｌ,相对标准偏差小于４％,采样频率为１２０次／ｈ。     

锰C-抗坏血酸甲醛-化学发光体系的研究

实验观察到锰 氧化抗坏血酸可以产生弱的化学发光 ,甲醛对这一化学发光反应有较强的增敏作用 ,据此建立了测定抗坏血酸的流动注射化学发光分析法。方法的检出限为 2× 1 0 -8mol/L抗坏血酸 ;线性响应范围为 6 .0× 1 0 -8～ 2 .0× 1 0 -5mol/L。对 1 .0× 1 0 -6mol/L的抗坏血酸进行 1 1次测定 ,相对标准偏差为 2 3%。该方法已成功应用于维生素C针剂和片剂中抗坏血酸含量的测定 ,结果与药典方法测得值一致     

反相高效液相色谱-增敏化学发光同时测定VB1和VC

本文基于维生素B1(VB1)、维生素C(VC)对鲁米诺(Luminol)和铁氰化钾(K3[Fe(CN)6])化学发光反应的增敏作用原理,建立了反相高效液相色谱(RP-HPLC)分离、柱后化学发光检测VB1与VC的新方法。当在鲁米诺中加入KBr时可以大大增敏该反应。本法已成功运用于蜂蜜和复合维生素片中VB1与VC的测定。     

非离子型微乳液介质-硫酸钡浊度法测定硫酸根

本文研究了以微乳液为介质,硫酸钡浊度法测定硫酸根离子的试验条件.以乳化剂OP/正丁醇/正庚烷/水四组分微乳液为介质,使硫酸钡颗粒分散均匀,显著提高了体系的稳定性,分析条件易于控制.本法选420nm为测定波长,硫酸根含量在50~500μg/25mL范围内成线性关系.本法具有简便、快速、准确等优点,用于水样和水泥样品的测定,结果令人满意.     

In Vitro Determination of Dobesilate in Medicine and Human Urine with Chemiluminescence Detection

A unique flow injection chemiluminescence (CL) method for the determination of calcium dobesilate in pharmaceutical preparations and human urine is presented in this paper. The analytical reagents involved in the CL reaction, luminol and ferricyanide, were both immobilized on an anion-exchange column in an FI system. The CL signal produced by the reaction of luminol with ferricyanide (the reagents had been eluted from the column through sodium phosphate injection) decreased in the presence of dobesilate. The decreased CL intensity was linear to the dobesilate concentration in the range 0.2100.0ngmL^–1. At a flow rate of 2.0mLmin^–1, one analytical cycle can be completed in 1.5min, including sampling and washing, resulting in a throughput of 40 cycles per hour. The proposed method was applied successfully to the determination of dobesilate in pharmaceutical preparations and human urine without any pre-treatment. It was found that, after oral administration, the dobesilate concentration reached its maximum after three hours, and the dobesilate metabolism ratio in 24 hours was 57.1% in the bodies of volunteers.Received September 14, 2002; accepted March 11, 2003 Published online July 16, 2003     

Determination of Tannic Acid by Flow Injection Analysis with Inhibited Chemiluminescence Detection

A novel flow injection procedure has been developed for the determination of tannic acid based on the inhibition of the chemiluminescences in luminol-H₂O₂-Manganese tetrasulfonatophthalocyanine (MnTSPc) system by tannic acid. The method is simple, rapid and sensitive with a detection limit of 8 × 10⁻¹⁰ mol·L⁻¹ and a linear range of 7 × 10⁻⁹–5 × 10⁻⁶ mol·L⁻¹. The relative standard deviation is 1.9% for eleven measurements of 5 × 10⁻⁷ mol·L⁻¹ tannic acid. The method has been successfully applied to the determination of tannic acid in real Chinese gall and hop pellets samples.     

Ultrasound,Acetic Acid,and Peracetic Acid as Alternatives Sanitizers to Chlorine Compounds for Fresh-Cut Kale Decontamination

Chlorinated compounds are usually applied in vegetable sanitization, but there are concerns about their application. Thus, this study aimed to evaluate ultrasound (50 kHz), acetic acid (1000; 2000 mg/L), and peracetic acid (20 mg/L) and their combination as alternative treatments to 200 mg/L sodium dichloroisocyanurate. The overall microbial, physicochemical, and nutritional quality of kale stored at 7 °C were assessed. The impact on Salmonella enterica Typhimurium was verified by plate-counting and scanning electron microscopy. Ultrasound combined with peracetic acid exhibited higher reductions in aerobic mesophiles, molds and yeasts, and coliforms at 35 °C (2.6; 2.4; 2.6 log CFU/g, respectively). Microbial counts remained stable during storage. The highest reduction in Salmonella occurred with the combination of ultrasound and acetic acid at 1000 mg/L and acetic acid at 2000 mg/L (2.8; 3.8 log CFU/g, respectively). No synergistic effect was observed with the combination of treatments. The cellular morphology of the pathogen altered after combinations of ultrasound and acetic acid at 2000 mg/L and peracetic acid. No changes in titratable total acidity, mass loss, vitamin C, or total phenolic compounds occurred. Alternative treatments presented equal to or greater efficacies than chlorinated compounds, so they could potentially be used for the decontamination of kale.     

流动注射化学发光法测定中药材中没食子酸

建立快速简便的流动注射化学发光分析法,用于中药材中没食子酸含量的测定.利用酸性介质中Fe3+-H2O2体系生成羟基自由基氧化没食子酸产生微弱的化学发光,用罗丹明6G来增敏化学发光.研究了影响化学发光的各种因素,探讨了可能的机理.结果表明,0.18 mol/L HCl,0.04 mol/L FeCl3,1.0 mol/L H2O2与1.0×10-4 mol/L罗丹明6G溶液组成最优的化学发光体系,没食子酸浓度在1.0×10-5～1.0×10-2 g/L和0.01～1.0 g/L范围内与化学发光强度呈很好的线性关系,r分别为0.9984和0.9947,检出限为3.0×10-6 g/L.对1.0×10-4 g/L没食子酸平行测定11次的相对标准偏差为3.8%.利用本方法成功地测定了中药材诃子和没食子中的没食子酸含量.     

单柱离子色谱法测定茶叶中草酸根和硫酸根的研究

本文研究单柱离子色谱分离测定茶叶中微量草酸根和硫酸根的方法。样品水浸泡，酸化液。上ＳｈｉｍＰａｒｓｋＩＣ－Ａ＿２柱分离，用２．０ｍｍｏｌ·Ｌ￣（－１）Ｈ－２Ｃ＿８Ｏ＿４／１．９ｍｍｏｌ·Ｌ￣（－１）Ｔｒｉ淋洗液洗脱，电导检测器检测，检测灵敏度为１．６Ｓ／ｃｍ，最低检出限０．０５μｇ／ｍＬ；线性范围Ｌ；相对标准偏差１．０６％；平均回收车９８．７２％９７．８８／。该法简便、快速、准确、灵敏、选择性好。