Solvent Evaporation Step Research Articles

Application of a novel ultra-low elution volume 96-well solid-phase extraction method to the LC/MS/MS determination of simvastatin and simvastatin acid in human plasma

A novel extraction method has been utilized in the LC/MS/MS determination of simvastatin and simvastatin acid in human plasma. In this method, 300 μl of plasma sample was loaded onto a Waters Oasis 96-well HLB μElution plate, the stationary phase was washed using 2 × 400 μl of 5% methanol in water, and the analytes were eluted using 35 μl of 95/5 acetonitrile/H 2O twice. The sample extracts were diluted with 40 μl of methyl ammonium acetate (1 mM, pH 4.5). Chromatography was performed on a Phenomenex Synergi Max-RP column (2.0 mm × 50 mm, 4 μm). A PE Sciex API 3000 tandem mass spectrometer interfaced with a turbo ionspray source was used for mass detection. Compared to solid-phase extraction, liquid–liquid extraction and solid-supported liquid–liquid extraction methods that were developed and previously used in our laboratory, this method reduced the labor cost and was less time consuming in sample preparation, due to the fact that post-extraction solvent evaporation and reconstitution steps were avoided using this μElution solid-phase extraction plate. The method has been proved to be fast, reliable and reproducible.

Design of pH-sensitive microspheres for the colonic delivery of the immunosuppressive drug tacrolimus

Recently, tacrolimus was shown to be effective in mitigating inflammatory bowel disease (IBD). In the treatment of IBD, oral drug delivery using pH-dependent polymers is one of the most successful therapeutic strategies. Eudragit P-4135F, a pH-sensitive polymer for colonic delivery was used to prepare tacrolimus microparticles using an oil/oil emulsification or an oil/water emulsification technique combined with a solvent extraction or evaporation step. Although the pH-dependent drug release was similar for all types of microspheres, it was generally found that encapsulation rates of oil/water systems (extraction 38.8±9.4%; evaporation 56.3±1.9%) were superior to the oil/oil emulsification (4.8±0.4%). Eudragit P-4135F was found to limit drug leakage at pH 6.8 to levels lower than 10% within 6 h. At pH 7.4, almost immediate release (within 30 min) was observed. From differential scanning calorimetry and X-ray analyses, the drug inside the polymeric microsphere matrix was concluded to be present in a molecular dispersion. Generally, all formulations proved their applicability in vitro as a promising device for pH-dependent colonic delivery of tacrolimus, however, the oil/water technique was found to be superior to the oil/oil approach and among them solvent evaporation seemed to be more advisable, due to the higher encapsulation rate.

Determination of Pesticide Residues in Nonfatty Fooda by Percritical Extraction aqnd Gas Chromatography/Mass Spectrometry: Collaborative Study

A collaborative study was conducted to determine multiple pesticide residues in apple, green bean, and carrot by using supercritical fluid extraction (SFE) and gas chromatography/mass spectrometry (GC/MS). Seventeen laboratories from 7 countries participated in the final study, and a variety of different instruments was used by collaborators. The procedure simply entails 3 steps: (1) mix 1.1 g drying agent (Hydromatrix) per 1 g frozen precomminuted sample, and load 4-5.5 g of this mixture into a 7-10 mL extraction vessel; (2) perform SFE for 20-30 min with a 1-2 mL/min flow rate of carbon dioxide at 0.85 g/mL density (320 atm, 60 degrees C); and (3) inject the extract, which was collected on a solid-phase or in a liquid trap, into the gas chromatograph/mass spectrometer, using either an ion-trap instrument in full-scan mode or a quadrupole-type instrument in selected-ion monitoring mode. The ability of GC/MS to simultaneously quantitate and confirm the identity of the semivolatile analytes at trace concentrations is a strong feature of the approach. The selectivity of SFE and GC/MS avoids the need for post-extraction cleanup steps, and the conversion of the CO2 solvent to a gas after SFE eliminates the solvent evaporation step common in traditional methods. The approach has several advantages, but its main drawback is the lower recoveries for the most polar analytes, such as methamidophos and acephate, and the most nonpolar analytes, such as pyrethroids. Recoveries for most pesticides are >75%, and recoveries of nonpolar analytes are still >50%. The (within-laboratory) repeatability relative standard deviation (RSDr) values of the recoveries are generally <15%. More specifically, the average results from the 9-14 laboratories in the final analysis of 6 blind duplicates at 3 concentrations for each pesticide are as follows: carbofuran in apple (75-500 ng/g), 89% recovery, 7% RSDr, 9% reproducibility relative standard deviation (RSDR); diazinon in apple (60-400 ng/g), 83% recovery, 13% RSDr, 17% RSDR; vinclozolin in apple (6-400 ng/g), 97% recovery, 13% RSDr, 18% RSDR; chlorpyrifos in apple (50-300 ng/g), 105% recovery, 11% RSDr, 13% RSDR; endosulfan sulfate in apple (150-1000 ng/g), 95% recovery, 15% RSDr, 17% RSDR; trifluralin in green bean (30-200 ng/g), 58% recovery, 11% RSDr, 27% RSDR; dacthal in green bean (60-400 ng/g), 88% recovery, 11% RSDr, 17% RSDR; quintozene in green bean (60-400 ng/g), 79% recovery, 13% RSDr, 18% RSDR; chlorpyrifos in green bean (50-300 ng/g), 84% recovery, 11% RSDr, 17% RSDR; p,p'-DDE in green bean (45-300 ng/g), 64% recovery, 14% RSDr, 27% RSDR; atrazine in carrot (75-500 ng/g), 90% recovery, 11% RSDr, 15% RSDR; metalaxyl in carrot (75-500 ng/g), 89% recovery, 8% RSDr, 12% RSDR; parathion-methyl in carrot (75-500 ng/g), 84% recovery, 14% RSDr, 15% RSDR; chlorpyrifos in carrot (50-300 ng/g), 77% recovery, 13% RSDr, 19% RSDR; and bifenthrin in carrot (90-600 ng/g), 63% recovery, 12% RSDr, and 25% RSDR. All analytes except for the nonpolar compounds trifluralin, p,p'-DDE, and bifenthrin gave average Horwitz ratios of <1.0 when AOAC criteria were used. These 3 analytes had high RSDr values but lower RSDR values, which indicated that certain SFE instruments gave consistently lower recoveries for nonpolar compounds. The collaborative study results demonstrate that the method meets the purpose of many monitoring programs for pesticide residue analysis, and the Study Director recommends that it be adopted Official First Action.

Improved sample preparation for the quantitative analysis of paroxetine in human plasma by stable isotope dilution negative ion chemical ionisation gas chromatography–mass spectrometry

An improved sample work-up and derivatisation procedure for the quantitative determination of paroxetine in human plasma by gas chromatography–negative ion chemical ionisation mass spectrometry is presented. Solvent extraction from plasma samples at alkaline pH was combined with derivatisation to the pentafluorobenzyl carbamate derivative in one step and subsequently analysed without any further purification. Thus, lengthy and time-consuming solvent evaporation steps are avoided to assure high-throughput analysis. Complete validation data are presented. The method is rugged, rapid and robust and has been applied to the batch analysis of paroxetine during pharmacokinetic profiling of the drug.

Efeito da adição de polietilenoglicóis nas formulações de microesferas de acetobutirato de celulose sobre a eficiência de encapsulação da carbamazepina e morfologia das partículas

With the aim of obtaining carbamazepine (CBZ) prolonged release dosage forms, cellulose acetate butyrate (CAB70) microspheres have been prepared by the emulsion/solvent evaporation method. In order to modulate the CBZ release, the addition of polyethylene glycols (PEG) in the internal phase of the emulsion was carried out. When compared with microspheres prepared only from CAB70, the encapsulation efficiency and the CBZ content were drastically reduced by the PEG 4000 addition. On the other hand, the incorporation of 10% (w/w) of PEG1500 did not affect the drug content in the microspheres. Most porous particles werw observed by SEM when PEG 1500 or 4000 was added to the formulations, however the lost of the spherical shape of the particles was verified when an ABC70:PEG 4000 1:1 mixture was used to prepare the microspheres. The addition of PEGs did not appear to affect the mean diameter of the particles. The decrease of the CBZ content was related to the PEG extraction during the solvent evaporation step and to its ability to dissolve the CBZ in the external phase of the emulsion. The porosity development control, by adjusting the amount or the molecular weight of PEG, can be useful in the drug release from microparticles.

Effect of Osmotic Pressure in the Solvent Extraction Phase on BSA Release Profile from PLGA Microspheres

This study investigated the influence of osmotic pressure in the organic solvent extraction phase on release profile of bovine serum albumin (BSA) from poly(lactide-co-glycolide) (PLGA) microspheres. BSA-loaded PLGA microspheres with a target load of 10% were prepared by a double emulsion phase separation method. All the microsphere batches were fabricated in the same conditions except that in the organic solvent (CH2Cl2) evaporation step. Different concentrations of NaCl (0, 1.8, and 3.6%) or sucrose (20%) were used to generate a range of osmotic pressures in the extraction aqueous phase. These microspheres were characterized for incorporation efficiency, surface and internal morphology, particle size, protein stability, and in vitro release. The microspheres were spherical with particle size ranging from 16.8 to 27.8 μm. Higher osmotic pressure resulted in a denser internal structure although similar nonporous surface morphology was observed with all batches. No significant difference in encapsulation efficiency existed from batch to batch (87–94%). Sodium dodecyl sulfate–polyamide gel electrophoresis showed that BSA integrity was well retained. The release profile of the batch prepared with only water as the continuous (solvent extraction) phase exhibited a 79% burst release in the first 24 hr followed by a plateau and then a little release after 21 days. In the presence of NaCl or sucrose, the burst effect significantly decreased with increase in osmotic pressure in the extraction aqueous phase, which was then followed by sustained release for 35 days. A mass balance was made when the release terminated. Therefore, in the organic solvent extraction and evaporation step, increasing the osmotic pressure in the aqueous phase both reduced the burst release from the microspheres and improved the subsequent sustained release profile.

Analysis of pesticide residues in eggs by direct sample introduction/gas chromatography/tandem mass spectrometry.

Direct sample introduction (DSI) or "dirty sample injection" is a rapid, rugged, and inexpensive approach to large volume injection in gas chromatography (GC) for semivolatile analytes such as pesticides. DSI of complex samples such as eggs requires a very selective detection technique, such as tandem mass spectrometry (MS-MS), to determine the analytes among the many semivolatile matrix components that also appear. In DSI, the nonvolatile matrix components that normally would contaminate the GC system in traditional injection methods remain in a disposable microvial, which is removed after every injection. For example, 3 microg of nonvolatile residue typically remained in the microvial after an injection of egg extract using the DSI method. This analytical procedure involves the following: (i) weighing 10 g of egg in a centrifuge tube and adding 2 g of NaCl and 19.3 mL of acetonitrile (MeCN); (ii) blending for 1 min using a probe blender; (iii) centrifuging for 10 min; and (iv) analyzing 10 microL (5 mg of egg equivalent) of the extract using DSI/GC/MS-MS. No sample cleanup or solvent evaporation steps were required to achieve quantitative and confirmatory results with <10 ng/g detection limits for 25 of 43 tested pesticides from several chemical classes. The remaining pesticides gave higher detection limits due to poor fragmentation characteristics in electron impact ionization and/or degradation. Analysis of eggs incurred with chlorpyrifos-methyl showed a similar trend in the results as a more traditional approach.

Long-term release of clodronate from biodegradable microspheres.

This paper describes the formulation of a biodegradable microparticulate drug delivery system containing clodronate, a bisphosphonate intended for the treatment of bone diseases. Microspheres were prepared with several poly(D,L-lactide-co-glycolide) (PLGA) copolymers of various molecular weights and molar compositions and 1 poly(D,L-lactide) (PDLLA) homopolymer by a water-in-oil-in-water (w/o/w) double emulsion solvent evaporation procedure. Critical process parameters and formulation variables (ie, addition of stabilizing agents) were evaluated for their effect on drug encapsulation efficiency and clodronate release rate from microparticles. Well-formed clodronate-loaded microspheres were obtained for all polymers by selecting suitable process parameters (inner water/oil volume ratio 1:16, temperature-raising rate in the solvent evaporation step 1 degree C/min, 2% wt/vol NaCl in the external aqueous phase). Good yields were obtained in all batches of clodronate microspheres (above 60%); drug encapsulation efficiencies ranged between 49% and 75% depending on the polymer used. Clodronate release from all copolymer microspheres was completed in about 48 hours, while those from PDLLA microspheres required about 20 days. The change of microsphere composition by adding a surfactant such as Span 20 or a viscosing agent such as carboxymethylcellulose extended the long-term release up to 3 months. Clodronate was successfully entrapped in PLGA and PDLLA microspheres, and drug release could be modulated from 48 hours up to 3 months by suitable selection of polymer, composition, additives, and manufacturing conditions.

Physico-chemical features and catalytic activity of sulfated zirconia prepared by sol-gel method. The role of the solvent evaporation step

ZrO2–SO4 powders have been prepared by following a single-step sol–gel preparative route using zirconium propoxide as the starting compound. Sulfuric acid was employed both as the sulfating agent and as the catalyst of the polycondensation reaction in the gel formation. Two different series of dried precursors were obtained by either evaporating the solvent in an oven at 100°C (xerogels) or in supercritical conditions (aerogels). All the samples were calcined at three temperatures (470, 550, and 630°C) for the same time length (5 h). The powders were characterized for phase composition–crystallinity, surface area–porosity, sulfur content and surface state (XPS). The catalytic activity of the calcined samples was tested in the isomerization of n-butane in a continuous system at 150°C in absence of H2 and 250°C in presence of H2. The role played by the conditions of the solvent elimination, at the end of the sol–gel reaction, in affecting the physico-chemical and catalytic properties of the powders is discussed.

Prevention of tricyclic antidepressant adsorption loss with diethylamine during solvent evaporation.

The authors evaluated the adsorption loss of tricyclic antidepressants in analytical procedures with solvent extraction and evaporation. In standard procedures with the use of triple solvent extraction between alkalinized and acidified samples before chromatographic analysis, the adsorption loss was more significant with the demethylated metabolites. As much as 50% adsorption loss can occur; this irreversible loss can be accounted for entirely during the solvent evaporation step. Because of differential adsorption loss among parent drugs, metabolites, and internal standards, the analytical methods usually had wide within-day and day-to-day variations. The authors found that the addition of as little as 0.05% diethylamine to the extract before evaporation completely eliminated the adsorption loss of amitriptyline-nortriptyline, imipramine-desipramine, and doxepin-desmethyldoxepin. with subsequent improvement in procedure performance. This simple modification can be adopted readily by all laboratories that use solvent extraction and subsequent chromatographic analysis of tricyclic antidepressants.

Process analysis, design, and control — a case study -

The problems of analysis, design, and control of industrial processes challenge the engineer to create a safe process with the desired functionality that meets both product quality and yield requirements. This paper describes a model based approach to analyze an existing production process (plant), to identify the potential benefits of optimizing the process for both yield and quality, to develop strategies exploit optimization opportunities by optimizing the design and applying advanced control techniques, and to support the implementation of the results into the production plant. The case study demonstrates that appropriate computer aided methods can significantly reduce both the time and cost required to improve the production compared with the traditional approach employing extensive pilot plant testing. The overall current production process consists of five main steps: a batch reaction, a dilution step, a continuous polymerization, solvent evaporation, and distillation step. However, this paper focuses on understanding and improving the first three steps. To develop a more profound theoretical understanding of the system and to formulate an adequate mathematical abstraction of the system, we developed rigorous models that viewed each stage in detail. Models of each task include the proper description continuous behavior of the system such as reaction schemes, material and energy balances, transport phenomena and kinetics; discrete operating alternatives for each step, such as employing a batch or continuous reactor, static or dynamic mixer, or melt or solution polymerization. Many experiments at laboratory scale are performed to get information about reaction order and velocity of the main and side reactions both in the melt and in solution. After establishing a set of appropriate models, additional experiments and available process measurements are used to validate the models. An analysis of the production process is carried out using these models, revealing some inefficiencies of the various subsystems of the plant and confirming the hypothesis that improvements to product quality and performance can be achieved by retrofitting the existing process. The task of designing a chemical plant can be viewed as a problem in which a number of specifications concerning the goals are translated into a set of specifications for the different process units while balancing the material and energy flows between them. In addition, design constraints are imposed to ensure plant operability, to reflect the availability of utilities, to ensure safe operation, to define the bounds on capital investment, etc. Dynamic simulation is used to evaluate and benchmark the design concepts considered; the performance of the process is assessed according to both economic benefit (net present value, cost reduction) and product quality, which is measured according to the amount of byproducts causing cross-links in the polymer and the often unavoidable formation of microgel. Once the optimal structure of the production process has been identified and design specifications for the each unit have been determined, the detailed design of the process is performed in a second step that is also based on computer simulation. This step includes both the design of vessels and pipes, which can be done relative easily, and the design of operation and control strategies, which pose challenging problems. All of these design steps within this case study, including a test of the system's performance, have been carried out using computer simulations that employ models verified by experiments on laboratory scale. This has enabled us to avoid constructing a pilot plant. In fact, some of the newly designed units have been directly incorporated and tested in the plant during a four month period, achieving satisfactory results as soon as they were implemented. Just eighteen months after starting this research project, management had been enabled to decide the implementation of the improved design into the production plant. Model based design and advanced control methods have advantages over traditional engineering practice, yet they are not without some deficiencies. In summary, model based design helps to reduce the number of experiments that must be conducted on laboratory scale and can avoid pilot plant construction.

Determination of retinol, alpha-tocopherol, alpha- and beta-carotene by direct extraction of human serum using high performance liquid chromatography.

In this report we describe a modified reverse phase HPLC method that avoids the solvent evaporation step and allows simple and rapid determination of retinol, alpha-tocopherol, alpha-carotene and beta-carotene and achieves complete separation of alpha- and beta-carotene. Retinyl acetate, alpha-tocopheryl acetate and retinyl palmitate in ethanol were added to serum as internal standards. Serum was then deproteinized with an equal volume of ethanol, and the lipid was extracted with ethyl acetate-butanol (1:1 v/v). A portion of this solution was injected into a C18 reverse phase chromatographic column and absorbencies of the vitamins and internal standards were measured at 292 nm for tocopherols, 325 nm for retinoids and 450 nm for carotenoids; peak-height ratios were used to quantify each vitamin. The analytical recoveries for retinol, alpha-tocopherol alpha- and beta-carotene at various concentrations tested were 95-103, 90-98, 92-99 and 94-96%, respectively. The intra- and interassay variations for low and high concentrations of retinol, alpha-tocopherol, alpha- and beta-carotene ranged from 2.4 to 6.7 for intraassay and from 4.3 to 8.5 for interassay replication. The detection limits were 1.25 (0.04), 19 (0.44), 0.35 (0.006) and 0.94 (0.017) micrograms/dL (delta mol/L) for retinol, alpha-tocopherol, alpha- and beta-carotene, respectively.

Automated sample preparation using membrane microtiter extraction for bioanalytical mass spectrometry

The development and application of membrane solid phase extraction (SPE) in 96-well microtiter plate format is described for the automated analysis of drugs in biological fluids. The small bed volume of the membrane allows elution of the analyte in a very small solvent volume, permitting direct HPLC injection and negating the need for the time consuming solvent evaporation step. A programmable liquid handling station (Quadra 96) was modified to automate all SPE steps. To avoid drying of the SPE bed and to enhance the analytical precision a novel protocol for performing the condition, load and wash steps in rapid succession was utilized. A block of 96 samples can now be extracted in 10 min., about 30 times faster than manual solvent extraction or single cartridge SPE methods. This processing speed complements the high-throughput speed of contemporary high performance liquid chromatography mass spectrometry (HPLC/MS) analysis. The quantitative analysis of a test analyte (Ziprasidone) in plasma demonstrates the utility and throughput of membrane SPE in combination with HPLC/MS. The results obtained with the current automated procedure compare favorably with those obtained using solvent and traditional solid phase extraction methods. The method has been used for the analysis of numerous drug prototypes in biological fluids to support drug discovery efforts. © 1997 John Wiley & Sons, Ltd.

Automated sample preparation using membrane microtiter extraction for bioanalytical mass spectrometry.

The development and application of membrane solid phase extraction (SPE) in 96-well microtiter plate format is described for the automated analysis of drugs in biological fluids. The small bed volume of the membrane allows elution of the analyte in a very small solvent volume, permitting direct HPLC injection and negating the need for the time consuming solvent evaporation step. A programmable liquid handling station (Quadra 96) was modified to automate all SPE steps. To avoid drying of the SPE bed and to enhance the analytical precision a novel protocol for performing the condition, load and wash steps in rapid succession was utilized. A block of 96 samples can now be extracted in 10 min., about 30 times faster than manual solvent extraction or single cartridge SPE methods. This processing speed complements the high-throughput speed of contemporary high performance liquid chromatography mass spectrometry (HPLC/MS) analysis. The quantitative analysis of a test analyte (Ziprasidone) in plasma demonstrates the utility and throughput of membrane SPE in combination with HPLC/MS. The results obtained with the current automated procedure compare favorably with those obtained using solvent and traditional solid phase extraction methods. The method has been used for the analysis of numerous drug prototypes in biological fluids to support drug discovery efforts.

Use of a keeper to enhance the recovery of volatile polycyclic aromatic hydrocarbons in HPLC analysis

The recorveries of volatile polycyclic aromatic hydrocarbons in HPLC analysis may be enhanced if a long-chain alcohol, e.g. 1-hexanol or 1-octanol, is used as keeper in the solvent-evaporation step. Even under the harsh conditions of the vacuum-concentrator centrifuge, recoveries of more than 90% were achieved for 14 of the 15 PAH tested. The use of liquid-liquid extraction (LLE) eliminates the problem of adsorption of highly condensed aromatics by the wall of the sampling bottle. The combination of LLE with vacuum-controlled rotary evaporation and use of a keeper yielded overall recoveries between 50 and 130%, for most substances close to 100%, from tap water spiked with trace concentrations.

Membrane Morphology—A Model Correlating Thickness of Membrane Surface Skin Layer with Solvent Evaporation Time

Abstract A simple model has been developed which relates membrane surface skin layer thickness to solvent evaporation time. This model can be used to determine other important membrane morphology parameters such as pore number (or pore density) in every pore size distribution on the membrane surface. With pore number becoming available, membrane morphology can now be more completely, explicitly, and quantitatively characterized. The changes in membrane morphology parameters during the solvent evaporation step of making cellulose acetate butyrate (CAB) membrane (in acetone) were investigated based on the Surface Force-Pore Flow (SFPF) model and a new model developed in this work. The analyses show that in the solvent evaporation step of making CAB membranes, there exist three distinct morphology stages or phases associated with solvent evaporation time: (I) intrinsic pore-determining phase, (II) phase of forming dominantly massive small pores, and (III) phase of forming dominantly large pores. It is the co...

Fully automated methods for the determination of hydrochlorothiazide in human plasma and urine.

LC assays utilizing fully automated sample preparation procedures on Zymark PyTechnology Robot and BenchMate Workstation for the quantification of hydrochlorothiazide (HCTZ) in human plasma and urine have been developed. After aliquoting plasma and urine samples, and adding internal standard (IS) manually, the robot executed buffer and organic solvent addition, liquid-liquid extraction, solvent evaporation and on-line LC injection steps for plasma samples, whereas, BenchMate performed buffer and organic solvent addition, liquid-liquid and solid-phase extractions, and on-line LC injection steps for urine samples. Chromatographic separations were carried out on Beckman Octyl Ultrasphere column using the mobile phase composed of 12% (v/v) acetonitrile and 88% of either an ion-pairing reagent (plasma) or 0.1% trifluoroacetic acid (urine). The eluent from the column was monitored with UV detector (271 nm). Peak heights for HCTZ and IS were automatically processed using a PE-Nelson ACCESS*CHROM laboratory automation system. The assays have been validated in the concentration range of 2-100 ng ml-1 in plasma and 0.1-20 micrograms ml-1 in urine. Both plasma and urine assays have the sensitivity and specificity necessary to determine plasma and urine concentrations of HCTZ from low dose (6.25/12.5 mg) administration of HCTZ to human subjects in the presence or absence of losartan.

Effects of Membrane-Making Conditions and Shrinkage Treatment on Morphology and Performance of Cellulose Acetate Butyrate Membranes

Abstract The functions of additives in cellulose acetate butyrate (CAB) membrane casting solution, effect of thermal shrinkage treatment on porous CAB membranes, and the changes of CAB membrane surface morphology during the solvent evaporation step have been investigated. Additives (glycerol and lactic acid) in CAB membrane casting solution function only as pore number promoting agents when used at low concentration and function both as pore number and pore size promoting agents when used at higher concentrations. Triethyl phosphate in CAB membrane casting solution functions both as a pore number promoting agent and as a secondary solvent for CAB. Three distinct phases can be observed in the solvent evaporation step in making CAB membranes. With the increase in solvent evaporation time, the number of pores in the first pore size distribution increases in the initial small pore-forming phase and decreases in the large pore-forming phase, and the number of pores in the second pore size distribution always increases with solvent evaporation time. These changes in pore numbers, pore sizes, and pore number ratio in two pore size distributions as well as the membrane skin layer thickness together govern the ultimate membrane performance and result in a maximum solute separation which, in the case of CAB/ acetone membranes, falls at 60 seconds of solvent evaporation time. Significant improvement of the performance of a porous CAB membrane can be achieved by thermal shrinkage treatment. Equally high CAB membrane performance can also be achieved by using a lower concentration of additives in the membrane casting solution.

On‐line liquid chromatography – gas chromatography for automated clean‐up and analysis of polycyclic aromatic hydrocarbons

AbstractA fully automated system, comprising a liquid chromatograph (LC) coupled on‐line to a gas chromatograph (GC) by means of a loop interface, has been constructed for clean‐up and analysis of polycyclic aromatic hydrocarbons (PAH). An autosampler was utilized for sample injection into the LC. By the use of a back‐flush technique in conjunction with an ordinary analytical aminopropylsilica column, PAH could be isolated by LC: a concurrent solvent evaporation injection technique was then used for on‐line transfer of the PAH fraction to the GC, where the PAH analysis was completed.Compared with ordinary off‐line LC clean‐up followed by GC analysis, the sensitivity has been increased by a factor of 50–100, yielding a detection limit for individual PAH of a few nanograms per sample when using flame ionization detection. Further, irreproducible losses of low molecular weight PAH as a result of solvent evaporation steps in off‐line clean‐up procedures have been eliminated. Reproducibility of retention times and relative peak areas is high, facilitating automatic peak identification and calculation of concentrations, and the system can thus be used for automatic sample evaluation. The total time required for clean‐up and analysis is only 1.5 hours, and the demand on personnel time for the analysis of PAH has been drastically reduced.The technique has been demonstrated with samples of urban air and of used automobile engine lubricating oil.

A rapid method for the determination of methoprene in tobacco by high performance liquid chromatography

A rapid sample preparation procedure combined with a short reversed-phase HPLC separation for the quantitation of methoprene residue in tobacco samples is described. A ground tobacco sample of 0.5 g is mixed with 3 mL of 2-propanol. The mixture is extracted for twelve minutes with the aid of sonication at an elevated temperature (45–55°C) and then filtered through a 0.45 μm disposable filter prior to injection on HPLC. No sample cleanup or solvent evaporation step is required. Chromatographic analysis is performed on a C-18 column and the analysis time is 12.5 minutes. The detection limit for methoprene in tobacco samples is one part per million (μg/g).