LIST developments at IGISOL

The ion guide technique was developed in Jyv?skyl? during the early 1980's. In the ion guide the reaction recoil products are stopped and thermalized in high purity helium gas where they remain ionic due to high ionization potential of helium atoms. Different designs of ion guide exist for light-ion induced fusion reactions, for heavy-ion induced fusion and for proton induced fission. Although the IGISOL method is fast and universal it is chemically unselective and in many cases relatively inefficient. In order to address these deficiencies in the technique, a new laser ion source project, FURIOS (Fast Universal Resonant laser Ion Source), commenced in 2004. In addition, resonance ionization spectroscopy has been tested off – line within a sextupole ion beam guide.     

HPLC method development and validation of cytotoxic agent phenyl‐heptatriyne in Bidens pilosa with ultrasonic‐assisted cloud point extraction and preconcentration

Extraction and pre‐concentration of a bioactive marker compound, phenyl‐1,3,5‐heptatriyne from Bidens pilosa, prior to HPLC has been demonstrated using both organic and ecofriendly solvents. Non‐ionic surfactants, viz. Triton X‐100, Triton X‐114 and Genapol X‐80, were used for extraction. No back‐extraction or liquid chromatographic steps were required to remove the target phytochemical from the surfactant‐rich extractant phase. The optimized cloud point extraction procedure has been shown to be a potentially useful methodology for the preconcentration of the target analyte, with a preconcentration factor of 4–99. Moreover, the method is simple, sensitive, rapid and consumes lesser solvent than traditional methods. An isocratic chromatographic separation and quantitation was accomplished on a C₁₈ column with acetonitrile–acidified aqueous as mobile phase at a flow rate of 1.0 mL/min, UV detection at 254 nm and specificity with photo diode‐array detector (PDA) and MS. Under the optimum experimental conditions recovery was satisfactory (99.18–100.33%) without interference from the surfactant. The method seems to be reliable with intraday precision and interday precision below 2.0%. Good linearity was obtained in the working range from 7.5 to 30 µg/mL with correlation coefficient >0.99. The limits of detection and quantitation were 1.84 and 6.13 µg/mL, respectively. The method was validated following international guidelines and successfully applied for quantitative assays of cytotoxic compound phenyl‐1,3,5‐heptatriyne in Bidens pilosa. Copyright © 2010 John Wiley & Sons, Ltd.     

Determination of cimetidine in human plasma by use of coupled-flow injection, solid-phase extraction, and capillary zone electrophoresis

Summary An on-line flow injection-solid-phase extraction-capillary zone electrophoresis (FI-SPE-CZE) method has been developed for determination of cimetidine in human plasma. Sodium dodecylsulfate (SDS) was used as dynamic chemical modifier for elimination of capillary contamination by biological macromolecules. FI on-line preconcentration and cleaning of the analyte by means of a C₁₈ microcolumn was performed automatically and CZE separation was performed consecutively without interruption of the applied voltage and between-run-washing of the capillary. A detection limit of 8 μgL⁻¹ (3×σ) was achieved at a sample throughput of 12h⁻¹. The approach was successfully used for a pharmacokinetic study of cimetidine.     

Trace-matrix separations for high-purity chromium,molybdenum and tungsten with cellulose collectors

Trace metals (20 elements) in high-purity chromium, molybdenum and tungsten are collected and preconcentrated by precipitation and adsorption on cellulose collectors. The compound methods allow the application of AAS and ICP-AES as determination methods for the production control of highly pure refractory metals under routine conditions.Presented in part at the 1989 European Winter Conference on Plasma Spectrochemistry, Reutte, Austria     

Investigation on the Decomposition of Carboplatin in Infusion Solutions

 An integrated solid-phase spectrophotometry/flow injection analysis (FIA) method is proposed for the determination of the synthetic colorant matter Ponceau 4R (P4R) in the presence of its unsulfonated derivative 2-hydroxy-1-[(naphthalenyl)azo] naphthalene (N2N). The procedure is based on the measurement of P4R at λ = 508, followed by retention and preconcentration of the low level concentration of N2N on a C₁₈ silica gel minicolumn and subsequent measurement of the absorbance of N2N at λ = 508 nm after its elution. The applicable concentration range, the detection and the relative standard were the following: for P4R, from 0.30 to 20.0 mg/L; 0.052 mg/L 1.1%; and for N2N, between 0.020 to 3.0 mg/L 0.003 mg/L and 1.1%. The method was applied to the determination of small amounts of N2N present in P4R in food and cosmetic products. Percentages of recovery between 95 and 105% were obtained in all instances. The method was applied satisfactorily to the determination of the compounds P4R and N2N in samples of sweets and cosmetic products when compared to results offered by a HPLC reference method. Received April 5, 2001. Revision July 25, 2001.     

二氧化钛紫外光在线消解测定COD的研究

以TiO2-K2Cr2O7协同光催化氧化体系为基础，结合流动注射分析方法建立了一种快速测定水样中化学需氧量（COD）的简便方法．该方法测试速度快，不需有毒、昂贵的试剂，具有广阔的应用前景．COD含量在10～100mg·L^-1和100～1000mg·L^-1范围内，吸光度与COD含量均呈良好的线性关系；测定30mg·L^-1和300mg·L^-1的COD标准溶液，RSD≤5．1％（n=7）；将本系统应用于实际环境水样测定，与国家标准分析方法测定结果相符．     

Automatic off/on-line preconcentration for ICP-OES: Powerful instrumentation for water analysis

Automated preconcentration techniques for off/on-line determination with ICP-OES have been developed for various metal ions of environmental interest. Preconcentration studies were performed on two different types of chemically bonded chelating ion-exchangers, namely EDTrA-cellulose (iminoacetate groups) and HSO₃ · oxine-cellulose. Enrichment studies were carried out at various preconcentration factors and also at different loadings.Presented in part at the 1989 European Winter Conference on Plasma Spectrochemistry, Reutte, Austria     

On‐line flow‐through extraction–preconcentration‐large volume injection‐RP LC for trace determination of pyrethroids in Slovak soil

A rapid micro‐analytical multiresidue method was developed for analysis of pyrethroids (kadethrin K, cypermethrin C and permethrin P) in soil micro‐sample (200 mg). It uses on‐line flow‐through extraction of soil micro‐samples (packed into a short glass column) with a methanol‐aqueous citric acid buffer mixture, successive on‐line SPE preconcentration of analytes from the extract and on‐line RP‐HPLC analysis with UV photometric detection. The separation of pyrethroids is performed on a Purospher RP‐18e column with methanol/water as mobile phase. Effects of sorbent placed at the bottom of a short column holding the soil sample and different kinds of on‐line SPE columns were tested. Besides, the influence of volume of the effluent on the pyrethroids recovery was also studied. Calibration curves were linear over the range assayed from 0.01 to 0.2 μg/mL with correlation coefficients of linear regression (least‐squares method) in the range 0.998–0.999. Recovery studies were carried out at 0.25–1.00 μg/g dry soil fortification level and obtained recoveries were for K 81–84%, C 56–59% and for P 58–63%. Achieved LOD (confidence band) of studied pyrethroids were for large‐volume injection (1 mL) 4.5 ng K, 3.7 ng C, 3.6 ng P or 27 ng/g K, 32 ng/g C and 29 ng/g P in dry soil “solid sampling HPLC”.     

Rapid and direct determination of glyphosate,glufosinate, and aminophosphonic acid by online preconcentration CE with contactless conductivity detection

Rapid and direct online preconcentration followed by CE with capacitively coupled contactless conductivity detection (CE‐C⁴D) is evaluated as a new approach for the determination of glyphosate, glufosinate (GLUF), and aminophosphonic acid (AMPA) in drinking water. Two online preconcentration techniques, namely large volume sample stacking without polarity switching and field‐enhanced sample injection, coupled with CE‐C⁴D were successfully developed and optimized. Under optimized conditions, LODs in the range of 0.01–0.1 μM (1.7–11.1 μg/L) and sensitivity enhancements of 48‐ to 53‐fold were achieved with the large volume sample stacking‐CE‐C⁴D method. By performing the field‐enhanced sample injection‐CE‐C⁴D procedure, excellent LODs down to 0.0005–0.02 μM (0.1–2.2 μg/L) as well as sensitivity enhancements of up to 245‐ to 1002‐fold were obtained. Both techniques showed satisfactory reproducibility with RSDs of peak height of better than 10%. The newly established approaches were successfully applied to the analysis of glyphosate, glufosinate, and aminophosphonic acid in spiked tap drinking water.     

三聚氰胺-甲醛-三乙烯四胺树脂的合成及其对痕量银的吸附性能研究与应用

以甲醛为交联剂,以三聚氰胺、三乙烯四胺为原料合成了一种新型的三聚氰胺-甲醛-三乙烯四胺(MF-TETA)分离树脂,研究了MF-TETA分离树脂对痕量银的分离富集性能,探讨了MF-TETA分离树脂对银的吸附原理与最佳条件。在pH6.0、温度为35℃的条件下,试液中的银可被MF-TETA树脂定量吸附,其静态饱和吸附容量为32 mg/g,吸附在树脂上的银可用10 mL0.05 mol/L HNO3完全洗脱,洗脱液中的银用火焰原子吸收光谱法(FAAS)测定。该法对银的检出限为16 ng/mL(3σ,n=11),线性范围为0.05~5mg/mL,RSD=2.2%,回收率在95.8%~102.0%之间,方法可用于中草药中痕量银的测定。