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1.
A selective and sensitive liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was developed for the quantitative determination of 1-(3-chloropropyl)-4-(3-chlorophenyl)piperazine HCl (CCP HCl) a process related impurity in trazodone. The method provided excellent sensitivity at a typical target analyte level of <0.1 ppm, when the API samples were prepared at 5.0 mg/mL. The CCP HCl sample was analyzed on a C18 symmetry (100 mm × 4.6 mm, 3.5 μm) column interfaced with a triple quadruple tandem mass spectrometer operated in a multiple reaction monitoring (MRM) mode. Positive electro spray ionization (ESI) was employed as the ionization source and the mobile phase used was 5.0 mM ammonium acetate–acetonitrile (30:70, v/v). The injection precision of the lowest concentration standards was excellent with %RSD-1.42%. The calibration curve showed good linearity over the concentration range of 0.03–1.5 ppm with a correlation coefficient of >0.9996. Limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.01 and 0.03 ppm, respectively. The developed method was validated as per ICH guidelines in terms of LOD, LOQ, linearity, precision, accuracy, specificity and robustness.  相似文献   

2.
The chlorine used as disinfectant in tap water degrades most materials, including polyethylene. The most adequate (functional) test method, the pressure test, is complicated and expensive because the chlorinated aqueous media (Cl2 or ClO2 in water) are unstable and they undergo reactions that are dependent on the pH. A new method which assesses the protection efficiency of phenolic antioxidants in polyolefins was developed. The method uses a liquid hydrocarbon analogue, squalane, in which antioxidants are dissolved. The organic phase was dispersed in the aqueous chlorinated phase (containing 10 ppm of either Cl2 or ClO2; pH = 6.8) at 70 °C by intense stirring. The depletion of antioxidant (Irganox 1010) was monitored by standard DSC determination of the oxidation induction time. It was shown that 300 min of exposure was sufficient to obtain useful data.  相似文献   

3.
A simple, rapid, precise, accurate and sensitive high performance liquid chromatographic method has been developed for simultaneous determination of ACE inhibitors with hydrochlorothiazide and indapamide in pharmaceutical formulations. ‘Design of Experiments’ (DoE) using ‘central composite design’ (CCD) was applied to facilitate method development and optimization. Mobile phase was optimized utilizing response surface methodology using Design Expert software. Chromatographic separation was achieved on Hypersil®-Gold C18 (100 × 4.6 mm, 3 μm, Thermo Fisher Scientific, USA), column at 25 °C. The mobile phase was 58% buffer (5 mM KH2PO4, containing triethylamine 0.25 ml/L), 25% acetonitrile and 17% methanol (pH adjusted to 2.8 ± 0.1). The analysis was performed at 215 nm. The mobile phase flow rate was 1.0 ml/min and injection volume 10 μl. The method was validated for linearity, limits of quantitation and detection, accuracy, precision, ruggedness and robustness as per the International Conference on Harmonization (ICH) guidelines. Calibration curves (for lisinopril, hydrochlorothiazide, captopril, imidapril, perindopril, indapamide and trandolapril) were linear in the concentration range of 5–35 μg/ml. The limit of detection and limit of quantitation for experimental drugs ranged from 0.03 to 0.61 and 0.08–1.84 μg/ml respectively.  相似文献   

4.
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.  相似文献   

5.
Food packaging polymers, polystyrene (PS), polycarbonate (PC), polyamide-6 (PA-6), and polyvinylchloride (PVC), were irradiated with dose in the range 5–200 kGy. The quantities of corresponding monomer residues (styrene monomer, bisphenol-A, ε-caprolactam, vinyl chloride) released from target materials were analyzed using a SIM mode of GC/MSD. Styrene monomer in PS showed a slight increase from 740 to 777 ppm at 5–30 kGy and then decreased as the dose increased from 30 to 200 kGy. Bisphenol-A in PC was dose independent at the low doses, 5, 10 and 30 kGy, but its level increased from 173 to 473 ppm at 30 kGy and thereafter remained unchanged through 200 kGy. ε-Caprolactam in PA-6 was also dose independent, in the range of 5–200 kGy, but its level (122–164 ppm) was found to be higher than those (71 ppm) of non-irradiated sample. As for PVC, the quantity of vinyl chloride tended to increase from 8 to 18 ppm at 5–200 kGy.  相似文献   

6.
Analytical performances of metal coated slotted quartz tube flame atomic absorption spectrometry (SQT-FAAS) and slotted quartz tube in situ atom trapping flame atomic absorption spectrometry (SQT-AT-FAAS) systems were evaluated for determination of Bi. Non-volatile elements such as Mo, Zr, W and Ta were tried as coating materials. It was observed that W-coated SQT gave the best sensitivity for the determination of Bi for SQT-FAAS and SQT-AT-FAAS. The parameters for W-coated SQT-FAAS and W-coated SQT-AT-FAAS were optimized. Sensitivity of FAAS for Bi was improved as 4.0 fold by W-coated SQT-FAAS while 613 fold enhancement in sensitivity was achieved by W-coated SQT-AT-FAAS using 5.0 min trapping with respect to conventional FAAS. MIBK was selected as organic solvent for the re-atomization of Bi from the trapping surface. Limit of detection values for W-coated SQT-FAAS and W-coated SQT-AT-FAAS was obtained as 0.14 μg mL 1 and 0.51 ng mL 1, respectively. Linear calibration plot was obtained in the range of 2.5–25.0 ng mL 1 for W-coated SQT-AT-FAAS. Accuracy of the W-coated SQT-AT-FAAS system was checked by analyzing a standard reference material, NIST 1643e.  相似文献   

7.
A simple, rapid high-performance liquid chromatographic (HPLC) method was developed for the simultaneous determination of glycolic acid, lactic acid, glicolide, lactide and ethyacetate in monomers for obtaining biopolymers. The separation was effected on the reversed-phase C18 column 250mm×4.6 mm with particle size 5 μ using a mobile phase mixture buffer and acetonitrile in a ratio 88:12 v/v and elution was isocratic at a flow-rate of 1.0 mL/min. The determinations were performed with a UV-Vis detector at 200 nm. The volume of the injected sample was 20 μL. Detection limits for acids and its dimers (glycolic acid, lactic acid, glicolide, lactide) and ethylacetate range between 82 and 182 ng/mL. The analytes are separated in 13 min. Recovery studies showed good results for all solutes (99–102%). The method is linear for all compounds over the concentration range tested, and shows good precision and accuracy, making it suitable for quantitation of acids and its dimers (glycolic acid, lactic acid, glicolide, lactide) and ethyl acetate in monomers.  相似文献   

8.
The intercalations of melamine into α- and γ-zirconium phosphates (α- and γ-ZrP) were investigated. Melamine-intercalated α-ZrP afforded two phases with different interlayer distances (d = 1.30 and 1.55 nm). The phase with d = 1.30 nm was obtained as the mixture with original α-ZrP at 30 min reaction by batch method, whereas the single phase with d = 1.55 nm was obtained by decantation method in saturated melamine aqueous solution. Contrary to this, for γ-ZrP a phase with d = 1.78 nm was obtained by both batch and decantation methods in saturated melamine aqueous solution. And new phase with d = 1.48 nm was formed in batch method at low pH or lower concentration of melamine aqueous solution. In these phases the arrangement of melamine changed from a monolayer structure to a bilayer structure with the increase of interlayer distance. Furthermore, melamine-intercalated α- and γ-ZrP adsorbed formaldehyde gas and formaldehyde in formalin solution by interacting with melamine molecule in the interlayer region. In melamine-intercalated γ-ZrP with d = 1.48 nm, the expansion of interlayer distance to around 1.6 nm was observed after the adsorption of formaldehyde gas and formaldehyde in formalin solution. The adsorption of formaldehyde in formalin solution was accompanied with the release of melamine in the interlayer region with increasing the concentration of formaldehyde at 65 °C.  相似文献   

9.
《Microchemical Journal》2011,97(2):324-329
Selenium (Se) is naturally occurring in the environment and is an essential nutrient in mammals. However, environmental Se can be increased to toxic levels through different industrial practices. The potential adsorption of the Se oxoanions, selenite and selenate, from aqueous solutions onto nanosynthesized MnFe2O4 was investigated using batch techniques and DRC-ICP-MS spectroscopy. The nanomaterial (NM) was laboratory synthesized through slow titration of a mixture of Fe2+ and Mn2+ ions. X-ray diffraction and Scherrer's equation were used to determine the phase of the material and crystallite size, respectively. The effects of pH, reaction time, competitive anions, and the adsorption capacity of the synthesized NM to bind selenite and selenate were investigated. The Langmuir isotherm was used to determine the binding capacity of the NM. Results showed that the phase of the nanomaterial was similar to Jacobsite with a size of 27.5 nm. Results also showed that the sorption of either 100 ppb of selenite or selenate was pH independent in the pH range 2 to 6 and occurred within 5 min of contact time. The introduction of Cl and NO3 anions individually added to solution had no significant effect on the sorption of either selenite or selenate. However, it was found that the addition of SO42 had a competitive effect only on the sorption of selenate, first seen at 10 ppm and more pronounced at 100 ppm of SO42. In the presence of 100 ppm of PO43, the adsorption of selenate decreased to 87% while selenite sorption decreased to 20%. From the Langmuir isotherm equation it was determined that the nano-Jacobsite had a selenite and selenate binding capacity of 6573.76 and 769.23 mg Se/kg of NM, respectively.  相似文献   

10.
A simple, specific and accurate isocratic RP-HPLC-DAD method was developed for the simultaneous determination of phenylephrine, paracetamol, caffeine and chlorpheniramine in bulk and tablet dosage form. The four contents are present in variable concentrations and have variable chromatographic behavior making the process of analysis very difficult. For present studies a reversed-phase C-18 column (150 mm × 4.5 mm i.d., particle size 5 μm) with mobile phase consisting of acetonitrile, methanol and 10 Mm phosphate buffer 16:22:62 (v/v) (pH of buffer 2.5 ± 0.02, adjusted with ortho phosphoric acid) was used. The flow rate was 1.0 ml/min and eluents were monitored at 280 nm. The mean retention times of phenylephrine, paracetamol, caffeine and chlorpheniramine were found to be 1.8, 3.1, 5.2 and 10.9 min, respectively. The method was validated in terms of linearity, range, specificity, accuracy, precision and robustness. The proposed method was successfully applied to the estimation of phenylephrine, paracetamol, caffeine and chlorpheniramine in combined tablet dosage form.  相似文献   

11.
Liquid phase extraction with back extraction (LPE-BE) combined with high performance liquid chromatography-diode array detection (HPLC-DAD) was applied for the extraction and determination of erythromycin A, B and C in fermentation broths. According to this procedure, the fermentation broth with the adjustment pH at a fixed value of 10 was first mixed with organic solvent (Vbroth/Vorg = 1.0). After shaking, the mixture was separated into two phases by microfuging at 13,000 rpm for 15 min. Then back extraction was performed into the acidic aqueous phase with pH 5.0 (Vorg/Vaq = 1.0). After centrifugation at 3000, the two phases were separated and 50 μL of the acidic aqueous phase was injected into the HPLC. The effects of different variables such as the nature of extraction solvent and the pH of samples and buffer were investigated. At the most appropriate conditions, dynamic linear ranges of 0.5–8, 0.1–0.9 and 0.1–0.9 mg mL−1 and limits of detection of 0.03, 0.003 and 0.002 mg mL−1 were obtained for erythromycin A, B and C, respectively. Relative standard deviations (RSDs) of the proposed method were less than 9.5%. The mean recoveries were 99.5%. The proposed method is simple and sensitive with highly clean-up effect and it can be used for monitoring the progress of erythromycin fermentation.  相似文献   

12.
The sensing characteristics to propene (C3H6) were examined at 600 °C under wet condition for the amperometric sensor using a yttria-stabilized zirconia (YSZ) tube and ZnO (+8.5 wt%Pt) sensing-electrode (SE). In order to improve the sensitivity to C3H6, the “pulsed-potential method” was adopted here. It was found that the current response varied almost linearly with C3H6 concentration in the range of 0–200 ppm when SE was polarized at +1.0 V (vs. Pt/air reference electrode) for a period of 0.3 s. By using the present “pulsed-potential method”, the sensitivity to 100 ppm C3H6 was increased about 1000 times, compared with the normal “constant-potential method”. The excellent selectivity to C3H6 was also obtained for the present sensor without influence of other hydrocarbons, NOx, CO, H2, etc.  相似文献   

13.
It is well recognized that calcium carbonates (CaCO3) is one of the main components of scale that is commonly encountered in chemical and related industries. The calcium carbonate scale often grows extensively on equipment and parts, causing major operational difficulties. This paper presents experiments on calcium carbonate scale formation and control in a piping system where the scale-forming solution flowed in a laminar manner: 30, 40, and 50 mL/min, respectively. Other parameters evaluated were: solution temperature (25, 30 and 40 °C), and concentrations of malic acid (C4H6O5) added as impurities (3.00 and 5.00 ppm). The scale-forming solution was made by mixing equimolar solutions of CaCl2 and Na2CO3, respectively. The scale formation process was monitored by measuring the conductivity of the solution coming out of the piping system. It was found that in all experiments, conductivity decreased abruptly after a certain induction period, during which time the conductivity remained steady. The induction period varied from 17 min to 34 min, which means that the scale starts forming 17 min to 34 min after the mixing of the solution. Higher flow rates resulted in more calcium carbonate scale mass, which indicate that the fluid flow enhances the scale formation. Similarly, increasing the temperature of the solution (25, 30, and 40 °C) resulted in the increase of the scale mass. Overall, higher malic acid concentrations resulted in longer induction time and less scale mass. Depending on the temperature and the malic acid concentration tested, the reduction in scale mass could be ≥ 200%. This drastic reduction in scale mass suggests that malic acid could be an effective anti-scalant for calcium carbonate scale. SEM imaging and its associated EDS analysis confirmed that the scale formed corresponds to that of calcite (CaCO3). The X-ray diffraction analysis of the scale showed that the scale consisted of crystalline matter which corresponds to the powder diffraction data for calcium carbonate. The addition of malic acid in trace amounts (0.00 to 5.00 ppm) was able to alter the morphology of the scale crystals, indicating the preference adsorption of malic acid on specific crystal surface.  相似文献   

14.
We previously reported biological safety of fullerene-C60 (C60) incorporated in liposome consisting of hydrogenated lecithin and glycine soja sterol, as Liposome-Fullerene (0.5% aqueous phase; a particle size, 76 nm; Lpsm-Flln), and its cytoprotective activity against UVA. In the present study, Lpsm-Flln was administered on the surface of three-dimensional human skin tissue model, rinsed out before each UVA-irradiation at 4 J/cm2, and thereafter added again, followed by 19-cycle-repetition for 4 days (sum: 76 J/cm2). UVA-caused corneum scaling and disruption of epidermis layer were detected by scanning electron microscopy. Breakdown of collagen type I/IV, DNA strand cleavage and pycnosis/karyorrhexis were observed in vertical cross-sections of UVA-irradiated skin models visualized with fluorescent immunostain or Hoechst 33342 stain. These skin damages were scarcely repressed by liposome alone, but appreciably repressed by Lpsm-Flln of 250 ppm, containing 0.75 ppm of C60-equivalent to a 1/3300-weight amount vs. the whole liposome. Upon administration with Lpsm-Flln [16.7 μM (12 ppm): C60-equivalent] on human abdomen skin biopsies mounted in Franz diffusion cells, C60 permeated after 24 h into the epidermis at 1.86 nmol/g tissue (1.34 ppm), corresponding to 0.3% of the applied amount and a 9.0-fold dilution rate, but C60 was not detected in the dermis by HPLC, suggesting no necessity for considering a toxicity of C60 due to systemic circulation via dermal veins. Thus Lpsm-Flln has a potential to be safely utilized as a cosmetic anti-oxidative ingredient for UVA-protection.  相似文献   

15.
A new and complete GC–ICP-MS method is described for direct analysis of trace metals in a gas phase process stream. The proposed method is derived from standard analytical procedures developed for ICP-MS, which are regularly exercised in standard ICP-MS laboratories. In order to implement the method, a series of empirical factors were generated to calibrate detector response with respect to a known concentration of an internal standard analyte. Calibrated responses are ultimately used to determine the concentration of metal analytes in a gas stream using a semi-quantitative algorithm. The method was verified using a traditional gas injection from a GC sampling valve and a standard gas mixture containing either a 1 ppm Xe + Kr mix with helium balance or 100 ppm Xe with helium balance. Data collected for Xe and Kr gas analytes revealed that agreement of 6–20% with the actual concentration can be expected for various experimental conditions.To demonstrate the method using a relevant “unknown” gas mixture, experiments were performed for continuous 4 and 7 hour periods using a Hg-containing sample gas that was co-introduced into the GC sample loop with the xenon gas standard. System performance and detector response to the dilute concentration of the internal standard were pre-determined, which allowed semi-quantitative evaluation of the analyte. The calculated analyte concentrations varied during the course of the 4 hour experiment, particularly during the first hour of the analysis where the actual Hg concentration was under predicted by up to 72%. Calculated concentration improved to within 30–60% for data collected after the first hour of the experiment. Similar results were seen during the 7 hour test with the deviation from the actual concentration being 11–81% during the first hour and then decreasing for the remaining period. The method detection limit (MDL) was determined for the mercury by injecting the sample gas into the system following a period of equilibration. The MDL for Hg was calculated as 6.8 μg · m 3. This work describes the first complete GC–ICP-MS method to directly analyze gas phase samples, and detailed sample calculations and comparisons to conventional ICP-MS methods are provided.  相似文献   

16.
Two simple and sensitive high performance liquid chromatographic (HPLC) methods have been developed for the simultaneous determination of three different quinolones: enrofloxacin, lomefloxacin and ofloxacin in their pure and dosage forms, one with reversed phase HPLC and the other with ion-pair HPLC. In reversed phase HPLC, method (A), the mobile phase consists of 2.18% aqueous solution of KH2PO4 with pH adjusted to 2.4 ± 0.2 with acetonitrile (80:20; v/v), the mobile phase pumped at flow rate of 1.2 ml min?1. A Neucleosil C18 column (10 μm, 100 Å), 250 mm length × 4.6 mm diameter was utilized as stationary phase. Detection was affected spectrophotometrically at 294 nm. While in ion-pair HPLC, method (B), the mobile phase was aqueous solution of 0.65% sodium perchlorate and 0.31% ammonium acetate adjusted to pH 2.2 ± 0.2 with orthophosphoric acid: acetonitrile (81:19; v/v), the mobile phase pumped at flow rate of 1.5 ml min?1. A μ bondapack C18 column (10 μm, 100 Å), 250 mm length × 4.6 mm diameter was utilized as stationary phase. Detection was affected spectrophotometrically at 294 nm. Linearity ranges for enrofloxacin, lomefloxacin and ofloxacin were 4.0–108, 7.0–112 and 8.0–113 μg ml?1, respectively using method A and 8.0–112, 7.0–112 and 5.0–105 μg ml?1, respectively applying method B. Minimum detection limits obtained were 0.013, 0.023 and 0.035 μg ml?1 for enrofloxacin, lomefloxacin and ofloxacin, respectively using method A, and 0.028, 0.023 and 0.011 μg ml?1 using method B. The proposed methods were further applied to the analysis of enrofloxacin in injection and tablets containing the ofloxacin and lomefloxacin drugs, and the results were satisfied.  相似文献   

17.
An HPTLC method for analysis of Exemestane in bulk and pharmaceutical formulation has been established and validated. The analyte was separated on aluminium plates precoated with silica gel 60 F254. The mobile phase was chloroform:methanol 9.2:0.8 (v/v). Quantification was done by densitometric scanning at 247 nm. Response was a linear function of Exemestane concentration in the range of 100–500 μg mL−1. The limit of detection and quantification for Exemestane were 5.8 and 17.58 μg mL−1, respectively. Average recovery of Exemestane was 100.1, which shows that the method was free from interference from excipients present in the formulation. The established method enabled accurate, precise, and rapid analysis of Exemestane in bulk as well as pharmaceutical formulation.  相似文献   

18.
A rapid, specific and sensitive multiresidue method based on dispersive solid phase extraction sample preparation and gas chromatography with the mass spectrometric detection for the analysis of 234 pesticides in Korean herbs (Acanthopanax senticosus, Morus alba L., Hovenia dulcis) has been developed. Method recoveries were found to be between 62 and 119% with relative standard deviation lower than 21% for all compounds in the concentration range of 0.05 to 0.400 mg kg? 1. Limits of quantification of most compounds are below 0.050 mg kg? 1. The data demonstrate that this method was successfully used for analysis of 234 pesticides in Korean herbs.  相似文献   

19.
A fast and sensitive procedure for extraction and preconcentration of molybdenum in plant samples based on solidified floating organic drop microextraction combined with flame atomic absorption spectrometry and discrete nebulization was developed. 8-Hydroxyquinoline (8-HQ) was used as complexing agent. The experimental conditions established were: 0.5% m v 1 of 8-HQ, 60 μL of 1-undecanol as the extractant phase, 2 min vortex extraction time, centrifugation for 2 min at 2000 rpm, 10 min into an ice bath and discrete nebulization by introducing 200 μL of solution. The calibration curve was linear from 0.02 to 4.0 mg L 1 with a limit of detection of 4.9 μg L 1 and an enhancement factor of 67. The relative standard deviations for ten replicate measurements of 0.05 and 1.0 mg L 1 Mo were 6.0 and 14.5%, respectively. The developed procedure was applied for determining molybdenum in corn samples and accuracy was proved using certified reference materials.  相似文献   

20.
The decomposition of volatile organic compounds (VOCs) using a pilot system of electron beam (EB)–catalyst coupling was investigated. Two aromatic VOCs, toluene (1800 ppmC) and o-xylene (1500 ppmC), were irradiated with a dose range of 0–10 kGy at room temperature. The removal efficiencies for toluene and o-xylene were 92.4% and 94.5%, respectively, under a 10 kGy absorbed dose condition, which were higher than the results of 45.7% and 52.3% when EB-only was used, respectively. The CO2 selectivity approached 100% for both toluene and o-xylene using the EB-catalyst coupling system, while the concentrations of O3 formed were 0.02 ppm (toluene) and 0.003 ppm (o-xylene) at 10 kGy. The aerosol concentration was also measured as 43.2 μg/m3 (toluene) and 53.4 μg/m3 (o-xylene) at 10 kGy absorbed dose.  相似文献   

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