用对磺基苯亚甲基硫代若丹宁为显色剂固相萃取光度法测定环境样品中痕量汞

合成了新试剂对磺基苯亚甲基硫代若丹宁(SBDTR),并用红外光谱、核磁共振氢谱和元素分析鉴定其结构.试验表明:在 pH 3.5 的 HOAc-NaOAc 缓冲介质中,吐温-80 存在下,SBDTR与汞反应生成 2:1 稳定络合物,该络合物可被 Waters Sep-Pak C,18 固相萃取小柱固相萃取,用乙醇洗脱后在乙醇介质中,在此络合物的吸收峰 550 nm 波长处测定其吸光度.体系的摩尔吸光率为 8.42×104L·mol-1·cm-1.汞的质量浓度在 0.1～4.0 mg·L-1 范围内符合比耳定律,应用于河水及食品试样中汞的测定,所得结果与原子吸收光谱法的测定结果相符.     

对氨基苯亚甲基硫代若丹宁固相萃取分离光度法测定环境水和食品样品中的铅

合成了新试剂对氨基苯亚甲基硫代若丹宁(ABTR),并用红外光谱、核磁共振氢谱和元素分析鉴定其结构。研究了ABTR与铅的显色反应,在pH3.8的HAc NaAc缓冲介质中,吐温80存在下,ABTR与铅反应生成2∶1稳定络合物,该络合物可被WatersSep PakC18小柱固相萃取,小柱上富集的络合物用乙醇洗脱后富集倍数可达50倍,在乙醇介质中,λmax=545nm,体系摩尔吸光系数ε=1.09×105L·mol-1·cm-1。铅量在0.05～4.0μg/mL内符合比尔定律,本法可用于环境水和食品样品中铅的测定。     

新试剂NSPAR固相萃取光度法测定氰化渣中铂的研究

在pH2.5的氯乙酸NaOH缓冲介质中,吐温80存在下,磺硝酚偶氮若丹宁(NSPAR)与铂反应生成2∶1稳定络合物,该络合物可被WatersSep PakC18小柱固相萃取,用氮氮二甲基甲酰氨(DMF)洗脱后用光度法测定。在洗脱液介质中,λmax=535nm,摩尔吸光系数ε=6.33×104L·mol-1·cm-1。铂质量浓度在0 001～0 080μg/mL内符合比尔定律,本方法可用于氰化渣中铂的测定。     

钯与对若丹宁偶氮苯甲酸络合物的固相萃取和光度测定

根据新试剂对若丹宁偶氮苯甲酸(RABA)与钯的显色反应及C18固相萃取小柱对显色络合物的固相萃取,建立了一种测定痕量钯的新方法,在pH为2.0～4.0的HCl-邻苯二甲酸氢钾(HCl-KHP)缓冲介质中,在CTMAB存在下,钯与RABA发生反应形成1:1的稳定络合物,该络合物可用C18固相萃取小柱富集,小柱上富集的络合物用乙醇洗脱后用光度法测定,在富集后的测定液中,络合物最大吸收波长为500 nm,摩尔吸光系数ε=1.36×105 L·mol-1·cm-1,Pd2 量在0.1～1.0 μg/mL内符合比尔定律,方法用于催化剂中钯的测定.     

固相萃取光度法测定食品中的微量汞

研究了氯磺酚偶氮硫代若丹宁(HSCT)与汞的显色反应,在pH 3.6的HAc-NaAc缓冲介质中,Triton X-100存在下,HSCT与汞反应生成21稳定络合物,该络合物可被C18固相萃取小柱定量萃取,小柱上保留的络合物用四氢呋喃洗脱后用分光光度法测定,λmax=550 nm,体系ε=9.64×104 L/mol/cm.汞含量在0～1.0μg/mL内符合比尔定律,方法可用于食品中痕量汞含量的测定.     

固相萃取光度法测定水样中的银

银是一种重要的环境元素,已被列为水质常规检测项目之一。本实验研究了氯磺酚偶氮硫代若丹宁[5-(2-羟基,4-磺酸基,5-氯苯-1-偶氮)-硫代若丹宁(HSCT)]与银的显色反应及C18固相萃取小柱对络合物的固相萃取,并基于此建立了一种用固相萃取光度法测定环境水样中μg／L级银含量的新方法。     

对磺酸基苯亚甲基若丹宁固相萃取光度法测定水中的汞

研究了对磺酸基苯基亚甲基若丹宁(SBDR)与汞的显色反应,在pH4.0的HAc NaAc缓冲介质中,吐温 80存在下,SBDR与汞反应生成2∶1稳定络合物,该络合物可被WatersPorapak Sep Park C18固相萃取小柱萃取,用乙醇洗脱后在乙醇介质中λmax=520nm,可用分光光度法测定,体系ε=1.16×105L/mol·cm。汞含量在0μg/mL～1.5μg/mL内符合比尔定律,方法可用于水样中汞含量的测定。     

对磺酸基苯亚甲基硫代若丹宁固相萃取光度法测定烟草添加剂中的汞

合成了新试剂对磺酸基苯亚甲基硫代若丹宁(SBDTR),并用红外光谱、核磁共振氢谱和元素分析鉴定其结构。研究了SBDTR与汞的显色反应。在pH3.5的HAc NaAc缓冲介质中,吐温 80存在下,SBDTR与汞反应生成2∶1稳定络合物。该络合物可用WatersSep ParkC18固相萃取柱萃取,用乙醇洗脱后,在乙醇介质中用分光光度法测定,体系摩尔吸光系数为8.36×104L·mol-1·cm-1。汞含量在0～4μg/mL内符合比耳定律。本方法可用于烟草添加剂中汞含量的测定,结果满意。     

对磺酸基苯亚甲基硫代若丹宁固相萃取光度法测定金的研究

用文献[4]合成的新试剂对磺酸基苯亚甲基硫代若丹宁(SBDTR),研究了SBDTR与金的显色反应。在HCl介质中,乳化剂-OP存在下,SBDTR与金反应生成2∶1稳定络合物,络合物的λmax=540 nm,ε=1.05×105L.mol-1.cm-1,金量在0.1~20μg/10 mL内符合比尔定律,样中的金用TBP萃淋树脂固相萃取柱分离和富集后用该方法测定,方法相对标准偏差为2.2%~3.6%,标准回收率为96%~105%。     

Using on-line solid phase extraction for flow-injection spectrophotometric determination of salbutamol

In the proposed procedure, the determination of salbutamol with Folin-Ciocalteau reagent (FC) using a flow injection analysis technique (FIA) with spectrophotometric detection at 750 nm is described. The lab-made FIA system consisted of a peristaltic pump Gilson Minipulse 3 equipped with Tygon tubes, double 6-port external Vici Valco sample injector and S 2000/SAD500 fiber optic spectrophotometer. It was controlled by a PC with use of originally compiled LabVIEW^®—supported software containing the mathematical library with various statistical functions for off-line data evaluation. Concentration, volume of reagents and flow rate were optimised by a simplex method. The proposed system was used for the direct determination of salbutamol sulphate in the tablets and the human urine without preliminary pre-treatment of the sample. The negative effect of interfering substances (excipients of the tablets and matrix of the urine) is overcome by a solid phase extraction (SPE), when salbutamol is adsorbed on the solid phase in the microcolumn, which is integrated directly into the flow system. Pre-treatment of the sample takes place directly in the flowing stream. The sample throughput without carryover of on-line SPE was 60-80 samples per hour. With the SPE column (Baker—carboxylic acid), salbutamol was determined in the linear range from 1 to 15 μg ml⁻¹ (R.S.D.=1.2%), with detection limit (3σ) 0.1 μg ml⁻¹ and a frequency of 40-60 samples per hour in the water solutions. The salbutamol was determined in the linear range from 2 to 20 μg ml⁻¹ (R.S.D.=1.7%), with detection limit (3σ) 1 μg ml⁻¹ and a frequency of 30 samples per hour in the samples of the human urine.     

2-(4-羧基苯偶氮)苯并噻唑固相萃取分光光度法测定铂的研究

根据新试剂2-(4-羧基苯偶氮)苯并噻唑(CPABT)与铂的显色反应及C8固相萃取小柱对显色络合物的固相萃取,建立了一种测定痕量铂的新方法,在pH为3.8~5.5的乙酸-乙酸钠缓冲介质中,在Tween-80存在下,铂与CPABT发生反应形成1∶1的稳定络合物,该络合物可用C8固相萃取小柱富集,小柱上富集的络合物用二甲基甲酰胺洗脱后用分光光度法测定,在富集后的测定液中,络合物最大吸收波长为508 nm,摩尔吸光系数ε=2.29×105L.mol-1.cm-1,Pt4 量在0.1~1.2μg/mL内符合比尔定律,方法已用于测定催化剂中的铂。     

固相萃取光度法测定烟草中的挥发酚

研究了用Waters Sep-Park-C18固相萃取小柱萃取测定烟草样品中的挥发酚的方法。用自动水蒸汽蒸馏仪蒸馏出烟草样品中的挥发酚，4-氨基安替比林显色，显色产物可用Waters Sep-Park-C18固相萃取小柱萃取，以乙醇洗脱后用分光光度法测定，该方法可用于烟草样品中挥发酚的测定。     

Study on the solid phase extraction and spectrophotometric determination of cobalt with 5-(2-benzothiazolylazo)-8-hydroxyquinolene

A highly sensitive, selective and rapid method for the determination of cobalt based on the rapid reaction of cobalt(II) with 5-(2-benzothiazolylazo)-8-hydroxyquinolene BTAHQ and the solid phase extraction of the Co(II)-BTAHQ complex with C18 membrane disks were developed. In the presence of pH = 6.4 buffer solution and cetylpyridenium chloride (CPC) medium, BTAHQ reacts with cobalt to form a deep violet complex with a molar ratio of 1:1 (cobalt to BTAHQ). This complex was enriched by the solid phase extraction with C18 membrane disks. An enrichment factor of 100 was obtained by elution of the complex from the disks with a minimal amount of isopentyl alcohol. In isopentyl alcohol medium, the molar absorptivity of the complex is 2.42 × 10⁵ L mol⁻¹ cm⁻¹ at 658 nm. Beer’s law is obeyed in the range of 0.01–0.38 μg mL⁻¹ in the measured solution. The relative standard deviation for 11 replicate samples of 0.20 μg mL⁻¹ level is 1.37%. The detection and quantification limits reach 3.1 and 9.7 ng mL⁻¹ in the original samples. This method was applied for the determination of cobalt in biological, water, soil and pharmaceutical preparation samples with good results.     

液液提取-固相萃取-气相色谱法测定牛肉中蝇毒磷残留量的研究

建立了液液提取-固相萃取-气相色谱火焰光度法(LLE-SPE-GC-FPD)测定牛肉中蝇毒磷的残留量.优化了气相色谱分离条件,研究了样品基质对蝇毒磷测定的影响,考察了Florisil固相萃取小柱和ODS固相萃取小柱的萃取效果,并选择乙酸乙酯为洗脱剂,考察了液-液提取和固相萃取的回收率.将该方法用于牛肉中蝇毒磷的测定,其检出限为0.02 μg/mL,回收率高于83%,相对标准偏差13.7%.使用气相色谱质谱仪(GC-MS)对样品中的蝇毒磷进行定性分析,其特征离子和相对丰度为362(100)、226(55)和210(40).     

Determination of chloroethenes in environmental biological samples using gas chromatography coupled with solid phase micro extraction

Summary An analytical method has been developed to determine the chloroethene series, tetrachloroethene (PCE), trichloroethene (TCE),cisdichloroethene (cis-DCE) andtransdichloroethene (trans-DCE) in environmental biotreatment studies using gas chromatography coupled with a solid phase micro extraction (SPME) technique. The volatile chlorinated compounds in aqueous solution can be analyzed directly without solvent extraction, purge and trap, or thermal heating. The calibration curves have demonstrated good linear relationships within 50.0 to 3000.0 g L^–1 concentration range. Detection limits are 18.0, 5.0, 25.0, and 42.0 g L^–1, for PCE, TCE,cis-DCE andtrans-DCE, respectively. Factors which affect the SPME process, such as sample adsorption time, thermal desorption time, and concentration of salt in the matrix, have also been evaluated.     

On-line molecularly imprinted solid phase extraction for the selective spectrophotometric determination of catechol

A molecularly imprinted polymer has been synthesized for a selective on-line catechol extraction, followed by its spectrophotometric determination in guarana powder, mate tea and tap water samples. A clean-up column, containing a methacrylic polymer + C₁₈ solid phase, was also used in order to enhance selectivity. The imprinted polymer was prepared by bulk polymerization using catechol as template and 4-vinylpyridine as the functional monomer. Permanganate solution was used as spectrophotometric reagent, where Mn(VII) was reduced to Mn(II) by catechol in an acid medium, causing color loss, which was monitored at 528 nm. Physical (extraction flow rate, elution flow rate, coil length) and chemical (nature and concentration of the eluent, potassium permanganate concentration) variables were optimized, and the selectivity was appraised using three molecules (4-chloro-2-methylphenol, 2-cresol, 2-methoxyphenol) similar to catechol. These molecules did not present interference in 1:8, 1:10 and 1:10 (catechol/concomitant) proportions, respectively. The analytical calibration curve ranged from 3.0 up to 100 μmol L^− 1 (r > 0.999; seven concentrations levels, n = 3) and the limits of detection (LOD) and quantification (LOQ) were 0.8 and 2.7 μmol L^− 1, respectively. Precision, expressed as RSD, was of 3.0% (20 μmol L^− 1, n = 10), and the analytical frequency was 15 h^− 1. Accuracy was checked by the HPLC technique and the results did not present significant difference at 95% confidence levels according to the t test.