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1.
Food Chem ; 328: 127113, 2020 Oct 30.
Article in English | MEDLINE | ID: mdl-32474239

ABSTRACT

In view of the high polarity and ubiquitous occurrence of perchlorate, achieving an ultra-trace analysis has become a challenging task. The present study aimed to develop a simple and generic pretreatment protocol based on cold-induced liquid-liquid extraction to efficiently extract perchlorate from tea and dairy products and remarkably decrease potential matrix interferences and laborious cleanup. By optimizing the pretreatment conditions, the enrichment factor of perchlorate increased by 7.79 times under the compromise between the matrix effect and extraction recovery. The validated method presented satisfactory selectivity, linearity, accuracy, precision, and matrix effect, providing recoveries of 78.2%-106.2% with RSDr ranging from 1.2% to 7.9% and RSDR less than 10.7% for tea and dairy products. This pretreatment protocol depended only on shaking, freezing, and centrifugation in one step, without additional equipment or tedious operations, which will be explored to a greater extent in complex biological or food matrices.


Subject(s)
Dairy Products/analysis , Food Analysis/methods , Food Contamination/analysis , Liquid-Liquid Extraction/methods , Perchlorates/analysis , Tea/chemistry , Centrifugation/methods , Cost-Benefit Analysis , Food Analysis/economics , Freezing , Liquid-Liquid Extraction/economics , Reproducibility of Results , Sensitivity and Specificity , Time Factors
2.
Drug Res (Stuttg) ; 69(6): 342-347, 2019 Jun.
Article in English | MEDLINE | ID: mdl-30658353

ABSTRACT

A sensitive, specific and cost-effective HPLC method was developed for quantitative determination of carbinoxamine in human plasma using liquid chromatography with ultraviolet detection. A simple liquid-liquid extraction by ethyl acetate was used to extract carbinoxamine from human plasma. Satisfactory separation was achieved by a mobile phase consisting of 20 mM ammonium dihydrogen orthophosphate containing 0.01% triethyl amine (pH adjusted to 3 by using phosphoric acid) and acetonitrile in ratio of (75:25, v/v) at a flow rate of 0.9 mL/min on Hypersil® BDS C18 column (250×4.6 mm, 5 µm) column. The UV detector was set at 260 nm. The developed method was validated in human plasma with a lower limit of quantitation of 5 ng/mL for carbinoxamine. Linearity was demonstrated over the concentration range 5-200 ng/mL. The observed within- and between-day assay precision ranged from 1.902 to 14.90%; accuracy varied between 98.87 and 108.0%. This method can be used suitably for pharmacokinetic studies and in therapeutic drug monitoring in patients treated with carbinoxamine.


Subject(s)
Drug Monitoring/methods , Histamine H1 Antagonists/blood , Liquid-Liquid Extraction/methods , Pyridines/blood , Administration, Oral , Adolescent , Chromatography, High Pressure Liquid/economics , Chromatography, High Pressure Liquid/methods , Cost-Benefit Analysis , Drug Monitoring/economics , Feasibility Studies , Healthy Volunteers , Histamine H1 Antagonists/administration & dosage , Histamine H1 Antagonists/pharmacokinetics , Humans , Limit of Detection , Liquid-Liquid Extraction/economics , Male , Pyridines/administration & dosage , Pyridines/pharmacokinetics , Reproducibility of Results , Sensitivity and Specificity , Spectrophotometry, Ultraviolet , Young Adult
3.
Mar Drugs ; 16(9)2018 Sep 11.
Article in English | MEDLINE | ID: mdl-30208611

ABSTRACT

The nutraceutical potential of microalgae boomed with the exploitation of new species and sustainable extraction systems of bioactive compounds. Thus, a laboratory-made continuous pressurized solvent extraction system (CPSE) was built to optimize the extraction of antioxidant compounds, such as carotenoids and PUFA, from a scarcely studied prokaryotic microalga, Gloeothece sp. Following "green chemical principles" and using a GRAS solvent (ethanol), biomass amount, solvent flow-rate/pressure, temperature and solvent volume-including solvent recirculation-were sequentially optimized, with the carotenoids and PUFA content and antioxidant capacity being the objective functions. Gloeothece sp. bioactive compounds were best extracted at 60 °C and 180 bar. Recirculation of solvent in several cycles (C) led to an 11-fold extraction increase of ß-carotene (3C) and 7.4-fold extraction of C18:2 n6 t (5C) when compared to operation in open systems. To fully validate results CPSE, this system was compared to a conventional extraction method, ultrasound assisted extraction (UAE). CPSE proved superior in extraction yield, increasing total carotenoids extraction up 3-fold and total PUFA extraction by ca. 1.5-fold, with particular extraction increase of 18:3 n3 by 9.6-fold. Thus, CPSE proved to be an efficient and greener extraction method to obtain bioactive extract from Gloeothece sp. for nutraceutical purposes-with low levels of resources spent, while lowering costs of production and environmental impacts.


Subject(s)
Carotenoids/isolation & purification , Cyanobacteria/chemistry , Dietary Supplements , Fatty Acids/isolation & purification , Green Chemistry Technology/methods , Microalgae/chemistry , Antioxidants/isolation & purification , Biological Products/isolation & purification , Biomass , Ethanol/chemistry , Green Chemistry Technology/economics , Liquid-Liquid Extraction/economics , Liquid-Liquid Extraction/methods , Temperature , Ultrasonic Waves
4.
Anal Bioanal Chem ; 410(20): 4967-4978, 2018 Aug.
Article in English | MEDLINE | ID: mdl-29947895

ABSTRACT

Benzodiazepines (BZD) and Z-hypnotics are frequently analyzed in forensic laboratories, and in 2012, the designer benzodiazepines (DBZD) emerged on the illegal drug scene. DBZD represent a particular challenge demanding new analytical methods. In this work, parallel artificial liquid membrane extraction (PALME) is used for sample preparation of DBZD, BZD, and Z-hypnotics in whole blood prior to UHPLC-MS/MS analysis. PALME of BZD, DBZD, and Z-hypnotics was performed from whole blood samples, and the analytes were extracted across a supported liquid membrane (SLM) and into an acceptor solution of dimethyl sulfoxide and 200 mM formic acid (75:25, v/v). The method was validated according to EMA guidelines. The method was linear throughout the calibration range (R2 > 0.99). Intra- and inter-day accuracy and precision, as well as matrix effects, were within the guideline limit of ± 15%. LOD and LLOQ ranged from 0.10 to 5.0 ng mL-1 and 3.2 to 160 ng mL-1, respectively. Extraction recoveries were reproducible and above 52%. The method was specific, and the analytes were stable in the PALME extracts for 4 and 10 days at 10 and - 20 °C. No carry-over was observed within the calibration range. PALME and UHPLC-MS/MS for the determination of DBZD, BZD, and Z-hypnotics in whole blood are a green and low-cost alternative that provides high sample throughput (96-well format), extensive sample clean-up, good sensitivity, and high reproducibility. The presented method is also the first method incorporating analysis of DBZD, BZD, and Z-hypnotics in whole blood in one efficient analysis. Graphical abstract.


Subject(s)
Benzodiazepines/blood , Chromatography, High Pressure Liquid/methods , Designer Drugs/analysis , Hypnotics and Sedatives/blood , Membranes, Artificial , Tandem Mass Spectrometry/methods , Benzodiazepines/analysis , Benzodiazepines/isolation & purification , Chromatography, High Pressure Liquid/economics , Designer Drugs/isolation & purification , Equipment Design , Humans , Hypnotics and Sedatives/analysis , Hypnotics and Sedatives/isolation & purification , Limit of Detection , Liquid-Liquid Extraction/economics , Liquid-Liquid Extraction/instrumentation , Tandem Mass Spectrometry/economics , Time Factors
5.
Trends Biotechnol ; 36(2): 216-227, 2018 02.
Article in English | MEDLINE | ID: mdl-29132753

ABSTRACT

Although microalgae are a promising biobased feedstock, industrial scale production is still far off. To enhance the economic viability of large-scale microalgae processes, all biomass components need to be valorized, requiring a multi-product biorefinery. However, this concept is still too expensive. Typically, downstream processing of industrial biotechnological bulk products accounts for 20-40% of the total production costs, while for a microalgae multi-product biorefinery the costs are substantially higher (50-60%). These costs are high due to the lack of appropriate and mild technologies to access the different product fractions such as proteins, carbohydrates, and lipids. To reduce the costs, simplified processes need to be developed for the main unit operations including harvesting, cell disruption, extraction, and possibly fractionation.


Subject(s)
Biotechnology/economics , Filtration/methods , Liquid-Liquid Extraction/methods , Microalgae/chemistry , Algal Proteins/isolation & purification , Biofuels/economics , Biomass , Biotechnology/methods , Carbohydrates/isolation & purification , Filtration/economics , Flocculation , Humans , Ionic Liquids/chemistry , Lipids/isolation & purification , Liquid-Liquid Extraction/economics , Microalgae/growth & development , Microalgae/isolation & purification , Microwaves , Sonication/economics , Sonication/methods
6.
Molecules ; 22(9)2017 Sep 11.
Article in English | MEDLINE | ID: mdl-28892008

ABSTRACT

(1) Background: Ionic liquids (ILs) are considered "green" solvents and have been widely used in the extraction and separation field in recent years; (2) Methods: In this study, some common ILs and functionalized magnetic ionic liquids (MILs) were used as adjuvants for the solvent extraction of paclitaxel from Taxus x media (T. x media) using methanol solution. The extraction conditions of methanol concentration, IL type and amount, solid-liquid ratio, extraction temperature, and ultrasonic irradiation time were investigated in single factor experiments. Then, three factors of IL amount, solid-liquid ratio, and ultrasonic irradiation time were optimized by response surface methodology (RSM); (3) Results: The MIL [C4MIM]FeCl3Br was screened as the optimal adjuvant. Under the optimization conditions of 1.2% IL amount, 1:10.5 solid-liquid ratio, and 30 min ultrasonic irradiation time, the extraction yield reached 0.224 mg/g; and (4) Conclusions: Compared with the conventional solvent extraction, this ultrasonic assisted extraction (UAE) using methanol and MIL as adjuvants can significantly improve the extraction yield, reduce the use of methanol, and shorten the extraction time, which has the potentiality of being used in the extraction of some other important bioactive compounds from natural plant resources.


Subject(s)
Antineoplastic Agents, Phytogenic/isolation & purification , Ionic Liquids/chemistry , Liquid-Liquid Extraction/methods , Paclitaxel/isolation & purification , Taxus/chemistry , Factor Analysis, Statistical , Hydrogen-Ion Concentration , Liquid-Liquid Extraction/economics , Methanol/chemistry , Plant Extracts/chemistry , Solvents/chemistry , Sonication , Temperature , Time Factors
7.
Rapid Commun Mass Spectrom ; 31(19): 1573-1581, 2017 Oct 15.
Article in English | MEDLINE | ID: mdl-28708331

ABSTRACT

RATIONALE: Transfluthrin is a relatively non-toxic rapid-acting synthetic pyrethroid insecticide. It is widely used in household and hygiene products. A sensitive and accurate bioanalytical method is required for quantification of its concentration in plasma and its potential target organ, the brain for studies to assess its health effects and toxicokinetics in mammals. METHODS: The samples were prepared by liquid-liquid extraction. Gas chromatography mass spectrometry (GC/MS) analysis was performed for the determination of transfluthrin in biological samples with an overall method run time of 15 min. Transfluthrin was quantified using selected-ion monitoring (SIM) in the negative chemical ionization (NCI) mode. Chromatographic separation was achieved using a Zebron® ZB5-MS GC column operating with 1 mL/min constant flow helium. Cis-Permethrin was used as the internal standard. RESULTS: The method was validated to be precise and accurate within the linear range of 1.0-400.0 ng/mL in plasma and 4.0-400.0 ng/mL in brain homogenate, based on a 100 µL sample volume for both matrices. This method was applied to samples following administration of a 10 mg/kg oral dose to male adult rats. The plasma concentrations were observed to be 11.70 ± 5.69 ng/mL and brain concentrations 12.09 ± 3.15 ng/g when measured 2 h post-dose. CONCLUSIONS: A rapid GC/NCI-MS method was demonstrated to be sensitive, specific, precise and accurate for the quantification of transfluthrin in rat plasma and brain. The optimized method was successfully used to quantify the rat plasma and brain concentrations of transfluthrin 2 h after the oral dosing of Sprague-Dawley rats.


Subject(s)
Brain Chemistry , Cyclopropanes/analysis , Cyclopropanes/blood , Fluorobenzenes/analysis , Fluorobenzenes/blood , Gas Chromatography-Mass Spectrometry/methods , Insecticides/analysis , Insecticides/blood , Administration, Oral , Animals , Cyclopropanes/administration & dosage , Fluorobenzenes/administration & dosage , Gas Chromatography-Mass Spectrometry/economics , Insecticides/administration & dosage , Liquid-Liquid Extraction/economics , Liquid-Liquid Extraction/methods , Male , Rats , Rats, Sprague-Dawley , Reproducibility of Results
8.
Anal Chem ; 89(2): 1155-1162, 2017 01 17.
Article in English | MEDLINE | ID: mdl-27958721

ABSTRACT

Circulating tumor cells (CTCs) have great potential to provide minimally invasive ways for the early detection of cancer metastasis and for the response monitoring of various cancer treatments. Despite the clinical importance and progress of CTC-based cancer diagnostics, most of the current methods of enriching CTCs are difficult to implement in general hospital settings due to complex and time-consuming protocols. Among existing technologies, size-based isolation methods provide antibody-independent, relatively simple, and high throughput protocols. However, the clogging issues and lower than desired recovery rates and purity are the key challenges. In this work, inspired by antifouling membranes with liquid-filled pores in nature, clog-free, highly sensitive (95.9 ± 3.1% recovery rate), selective (>2.5 log depletion of white blood cells), rapid (>3 mL/min), and label-free isolation of viable CTCs from whole blood without prior sample treatment is achieved using a stand-alone lab-on-a-disc system equipped with fluid-assisted separation technology (FAST). Numerical simulation and experiments show that this method provides uniform, clog-free, ultrafast cell enrichment with pressure drops much less than in conventional size-based filtration, at 1 kPa. We demonstrate the clinical utility of the point-of-care detection of CTCs with samples taken from 142 patients suffering from breast, stomach, or lung cancer.


Subject(s)
Cell Separation/instrumentation , Microfluidic Analytical Techniques/instrumentation , Neoplasms/pathology , Neoplastic Cells, Circulating/pathology , Cell Line, Tumor , Cell Separation/economics , Cell Separation/methods , Cell Size , Equipment Design , Humans , Liquid-Liquid Extraction/economics , Liquid-Liquid Extraction/instrumentation , Liquid-Liquid Extraction/methods , Microfluidic Analytical Techniques/economics , Microfluidic Analytical Techniques/methods , Neoplasms/blood , Time Factors
9.
J Sep Sci ; 40(1): 203-212, 2017 01.
Article in English | MEDLINE | ID: mdl-27759332

ABSTRACT

In pesticide residue analysis, relatively low-sensitivity traditional detectors, such as UV, diode array, electron-capture, flame photometric, and nitrogen-phosphorus detectors, have been used following classical sample preparation (liquid-liquid extraction and open glass column cleanup); however, the extraction method is laborious, time-consuming, and requires large volumes of toxic organic solvents. A quick, easy, cheap, effective, rugged, and safe method was introduced in 2003 and coupled with selective and sensitive mass detectors to overcome the aforementioned drawbacks. Compared to traditional detectors, mass spectrometers are still far more expensive and not available in most modestly equipped laboratories, owing to maintenance and cost-related issues. Even available, traditional detectors are still being used for analysis of residues in agricultural commodities. It is widely known that the quick, easy, cheap, effective, rugged, and safe method is incompatible with conventional detectors owing to matrix complexity and low sensitivity. Therefore, modifications using column/cartridge-based solid-phase extraction instead of dispersive solid-phase extraction for cleanup have been applied in most cases to compensate and enable the adaptation of the extraction method to conventional detectors. In gas chromatography, the matrix enhancement effect of some analytes has been observed, which lowers the limit of detection and, therefore, enables gas chromatography to be compatible with the quick, easy, cheap, effective, rugged, and safe extraction method. For liquid chromatography with a UV detector, a combination of column/cartridge-based solid-phase extraction and dispersive solid-phase extraction was found to reduce the matrix interference and increase the sensitivity. A suitable double-layer column/cartridge-based solid-phase extraction might be the perfect solution, instead of a time-consuming combination of column/cartridge-based solid-phase extraction and dispersive solid-phase extraction. Therefore, replacing dispersive solid-phase extraction with column/cartridge-based solid-phase extraction in the cleanup step can make the quick, easy, cheap, effective, rugged, and safe extraction method compatible with traditional detectors for more sensitive, effective, and green analysis.


Subject(s)
Chemistry Techniques, Analytical/economics , Chemistry Techniques, Analytical/instrumentation , Pesticide Residues/analysis , Chromatography, Gas/economics , Chromatography, Gas/instrumentation , Chromatography, Liquid/economics , Chromatography, Liquid/instrumentation , Crops, Agricultural/chemistry , Liquid-Liquid Extraction/economics , Liquid-Liquid Extraction/instrumentation , Solid Phase Extraction/economics , Solid Phase Extraction/instrumentation
10.
Sci Rep ; 6: 38368, 2016 12 06.
Article in English | MEDLINE | ID: mdl-27922073

ABSTRACT

The RNAzol RT reagent was used to provide pure RNA from human cells. We develop a protocol using RNAzol RT reagent to extract pure RNA from plants tissues and demonstrate that this RNA extraction method works not only at room temperature but also at elevated temperatures and provides the simplest and most effective single-step method to extract pure and undegraded RNA directly from tropical plants in the field. RNA extraction directly in a complex field environment opens up the way for studying gene-environment interactions at transcriptome level to decipher the complex regulatory network involved in multiple-stress responses.


Subject(s)
Coffea/chemistry , Fruit/chemistry , Liquid-Liquid Extraction/methods , Plant Leaves/chemistry , Plant Roots/chemistry , RNA, Plant/isolation & purification , Humans , Liquid-Liquid Extraction/economics , Manihot/chemistry , Oryza/chemistry , Reproducibility of Results , Temperature , Zea mays/chemistry
11.
Biotechnol Prog ; 32(4): 971-7, 2016 07 08.
Article in English | MEDLINE | ID: mdl-27390294

ABSTRACT

Mitigating the effect of fermentation inhibitors in bioethanol plants can have a great positive impact on the economy of this industry. Liquid-liquid extraction (LLE) using ethyl acetate is able to remove fermentation inhibitors-chiefly, acetic acid-from an aqueous solution used to produce bioethanol. The fermentation broth resulting from LLE has higher performance for ethanol yield and its production rate. Previous techno-economic analyses focused on second-generation biofuel production did not address the impact of removing the fermentation inhibitors on the economic performance of the biorefinery. A comprehensive analysis of applying a separation system to mitigate the fermentation inhibition effect and to provide an analysis on the economic impact of removal of acetic acid from corn stover hydrolysate on the overall revenue of the biorefinery is necessary. This study examines the pros and cons associated with implementing LLE column along with the solvent recovery system into a commercial scale bioethanol plant. Using details from the NREL-developed model of corn stover biorefinery, the capital costs associated with the equipment and the operating cost for the use of solvent were estimated and the results were compared with the profit gain due to higher ethanol production. Results indicate that the additional capital will add 1% to the total capital and manufacturing cost will increase by 5.9%. The benefit arises from the higher ethanol production rate and yield as a consequence of inhibitor extraction and results in a $0.35 per gallon reduction in the minimum ethanol selling price (MESP). © 2016 American Institute of Chemical Engineers Biotechnol. Prog., 32:971-977, 2016.


Subject(s)
Acetic Acid/isolation & purification , Liquid-Liquid Extraction/economics , Acetic Acid/chemistry , Acetic Acid/pharmacology , Biofuels , Ethanol/chemistry , Ethanol/metabolism , Fermentation/drug effects , Zea mays/chemistry , Zea mays/metabolism
12.
Article in English | MEDLINE | ID: mdl-27294531

ABSTRACT

A simple liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was firstly developed and validated for simultaneous determination of netupitant and palonosetron in human plasma using ibrutinib as the internal standard (IS). Following liquid-liquid extraction, the compounds were eluted isocratically on a Phenomenex C18 column (50mm×2.0mm, 3µm) with the mobile phase consisting of acetonitrile and 10mM ammonium acetate buffer (pH 9.0) (89:11, v/v) at the flow rate of 0.3mL/min. The monitored ion transitions were m/z 579.5→522.4 for netupitant, m/z 297.3→110.2 for palonosetron and m/z 441.2→138.1 for IS. Chromatographic run time was 2.5min per injection, which made it possible to analyze more than 300 of samples per day. The assay exhibited a linear dynamic range of 5-1000ng/mL for netupitant and 0.02-10ng/mL for palonosetron in plasma. The values for both within- and between-day precision and accuracy were well within the generally accepted criteria for analytical methods (<15%). Selectivity, linearity, lower limit of quantification (LLOQ), accuracy, precision, stability, matrix effect, recovery and carry-over effect were evaluated for all analytes. The method is simple, rapid, and has been applied successfully to a pharmacokinetic study of netupitant and palonosetron in healthy volunteers.


Subject(s)
Antiemetics/blood , Chromatography, High Pressure Liquid/methods , Isoquinolines/blood , Pyridines/blood , Quinuclidines/blood , Serotonin Antagonists/blood , Tandem Mass Spectrometry/methods , Chromatography, High Pressure Liquid/economics , Humans , Limit of Detection , Liquid-Liquid Extraction/economics , Liquid-Liquid Extraction/methods , Palonosetron , Tandem Mass Spectrometry/economics , Time Factors
13.
Bioanalysis ; 8(10): 1021-34, 2016 May.
Article in English | MEDLINE | ID: mdl-27079811

ABSTRACT

AIM: There is an ever-increasing demand for high-throughput LC-MS/MS bioanalytical assays to support drug discovery and development. RESULTS: Matrix effects of sofosbuvir (protonated) and paclitaxel (sodiated) were thoroughly evaluated using high-throughput chromatography (defined as having a run time ≤1 min) under 14 elution conditions with extracts from protein precipitation, liquid-liquid extraction and solid-phase extraction. A slight separation, in terms of retention time, between underlying matrix components and sofosbuvir/paclitaxel can greatly alleviate matrix effects. CONCLUSION: High-throughput chromatography, with proper optimization, can provide rapid and effective chromatographic separation under 1 min to alleviate matrix effects and enhance assay ruggedness for regulated bioanalysis.


Subject(s)
Antineoplastic Agents, Phytogenic/blood , Antiviral Agents/blood , Chromatography, High Pressure Liquid/methods , Paclitaxel/blood , Sofosbuvir/blood , Tandem Mass Spectrometry/methods , Animals , Antineoplastic Agents, Phytogenic/isolation & purification , Antiviral Agents/isolation & purification , Chromatography, High Pressure Liquid/economics , High-Throughput Screening Assays/economics , High-Throughput Screening Assays/methods , Humans , Liquid-Liquid Extraction/economics , Liquid-Liquid Extraction/methods , Paclitaxel/isolation & purification , Sofosbuvir/isolation & purification , Solid Phase Extraction/economics , Solid Phase Extraction/methods , Tandem Mass Spectrometry/economics
14.
Biomed Chromatogr ; 30(4): 618-24, 2016 Apr.
Article in English | MEDLINE | ID: mdl-26385597

ABSTRACT

A rapid and sensitive LC-MS/MS method was developed for the determination of linarin in small-volume rat plasma and tissue sample. Sample preparation was employed by the combination of protein precipitation (PPT) and liquid-liquid extraction (LLE) to allow measurement over a 5-order-of-magnitude concentration range. Fast chromatographic separation was achieved on a Hypersil Gold column (100 × 2.1 mm i.d., 5 µm). Mass spectrometric detection was achieved using a triple-quadrupole mass spectrometer equipped with an electrospray ionization interface operating in positive ionization mode. Quantification was performed using selected reaction monitoring of precursor-product ion transitions at m/z 593 → 285 for linarin and m/z 447 → 271 for baicalin (internal standard). The total run time was only 2.8 min per sample. The calibration curves were linear over the concentration range of 0.4-200 µg/mL for PPT and 0.001-1.0 µg/mL for LLE. A lower limit of quantification of 1.0 ng/mL was achieved using only 20 µL of plasma or tissue homogenate. The intra- and inter-day precisions in all samples were ≤14.7%, while the accuracy was within ±5.2% of nominal values. The validated method has been successfully applied to pharmacokinetic and tissue distribution study of linarin.


Subject(s)
Chromatography, High Pressure Liquid/methods , Glycosides/pharmacokinetics , Tandem Mass Spectrometry/methods , Animals , Chromatography, High Pressure Liquid/economics , Cirsium/chemistry , Glycosides/blood , Glycosides/isolation & purification , Limit of Detection , Liquid-Liquid Extraction/economics , Liquid-Liquid Extraction/methods , Male , Rats , Rats, Sprague-Dawley , Tandem Mass Spectrometry/economics , Tissue Distribution
15.
Methods Mol Biol ; 1383: 125-31, 2016.
Article in English | MEDLINE | ID: mdl-26660182

ABSTRACT

Drug screening is an essential component of clinical toxicology laboratory service. Some laboratories use only automated chemistry analyzers for limited screening of drugs of abuse and few other drugs. Other laboratories use a combination of various techniques such as immunoassays, colorimetric tests, and mass spectrometry to provide more detailed comprehensive drug screening. Mass spectrometry, gas or liquid, can screen for hundreds of drugs and is often considered the gold standard for comprehensive drug screening. We describe an efficient and rapid gas chromatography/mass spectrometry (GC/MS) method for comprehensive drug screening in urine which utilizes a liquid-liquid extraction, sample concentration, and analysis by GC/MS.


Subject(s)
Gas Chromatography-Mass Spectrometry/methods , Substance Abuse Detection/methods , Urinalysis/methods , Gas Chromatography-Mass Spectrometry/economics , Humans , Liquid-Liquid Extraction/economics , Liquid-Liquid Extraction/methods , Substance Abuse Detection/economics , Time Factors , Urinalysis/economics
16.
Biotechnol Prog ; 32(1): 126-33, 2016.
Article in English | MEDLINE | ID: mdl-26561271

ABSTRACT

Uricase is the enzyme responsible for the breakdown of uric acid, the key molecule leading to gout in humans, into allantoin, but it is absent in humans. It has been produced as a PEGylated pharmaceutical where the purification is performed through three sequential chromatographic columns. More recently an aqueous two-phase system (ATPS) was reported that could recover Uricase with high yield and purity. Although the use of ATPS can decrease cost and time, it also generates a large amount of waste. The ability, therefore, to recycle key components of ATPS is of interest. Economic modelling is a powerful tool that allows the bioprocess engineer to compare possible outcomes and find areas where further research or optimization might be required without recourse to extensive experiments and time. This research provides an economic analysis using the commercial software BioSolve of the strategies for Uricase production: chromatographic and ATPS, and includes a third bioprocess that uses material recycling. The key parameters that affect the process the most were located via a sensitivity analysis and evaluated with a Monte Carlo analysis. Results show that ATPS is far less expensive than chromatography, but that there is an area where the cost of production of both bioprocesses overlap. Furthermore, recycling does not impact the cost of production. This study serves to provide a framework for the economic analysis of Uricase production using alternative techniques.


Subject(s)
Chromatography/economics , Liquid-Liquid Extraction/economics , Urate Oxidase/isolation & purification , Humans , Monte Carlo Method , Polyethylene Glycols/chemistry , Software , Urate Oxidase/biosynthesis , Urate Oxidase/chemistry
17.
Biomed Chromatogr ; 30(4): 503-7, 2016 Apr.
Article in English | MEDLINE | ID: mdl-26207321

ABSTRACT

Cucurbitacin B (CuB), one of the most abundant forms of cucurbitacins, is a promising natural anticancer drug candidate. Although the anticancer activity of CuB has been well demonstrated, information regarding the pharmacokinetics is limited. A rapid, selective and sensitive UPLC-MS/MS for CuB was developed and validated using hemslecin A (HeA) as internal standard (IS). Plasma samples were pre-treated by liquid-liquid extraction with dichloromethane. Separation was achieved on a reversed-phase C18 column (50 × 4.6 mm, 5 µm) at 35°C using isocratic elution with water-methanol (25:75, v/v) at a flow rate of 0.3 mL/min. The analytes were monitored by a triple quadrupole tandem mass spectrometer with positive electrospray ionization mode. The calibration curve was linear (r > 0.995) in a concentration range of 0.3-100 ng/mL with a limit of quantification of 0.3 ng/mL. Intra- and inter-day accuracy and precision were validated by percentage relative error and relative standard deviation, respectively, which were both lower than the limit of 15%. This assay was successfully applied to a pharmacokinetic study of CuB in Wistar rats.


Subject(s)
Anti-Inflammatory Agents/blood , Chromatography, High Pressure Liquid/methods , Tandem Mass Spectrometry/methods , Triterpenes/blood , Animals , Anti-Inflammatory Agents/isolation & purification , Chromatography, High Pressure Liquid/economics , Cucurbitaceae/chemistry , Limit of Detection , Liquid-Liquid Extraction/economics , Liquid-Liquid Extraction/methods , Male , Rats, Wistar , Reproducibility of Results , Spectrometry, Mass, Electrospray Ionization/methods , Tandem Mass Spectrometry/economics , Triterpenes/isolation & purification
18.
Int J Mol Sci ; 16(4): 8430-53, 2015 Apr 15.
Article in English | MEDLINE | ID: mdl-25884332

ABSTRACT

The present study was designed to evaluate the performance of alternative bio-based solvents, more especially 2-methyltetrahydrofuran, obtained from crop's byproducts for the substitution of petroleum solvents such as hexane in the extraction of fat and oils for food (edible oil) and non-food (bio fuel) applications. First a solvent selection as well as an evaluation of the performance was made with Hansen Solubility Parameters and the COnductor-like Screening MOdel for Realistic Solvation (COSMO-RS) simulations. Experiments were performed on rapeseed oil extraction at laboratory and pilot plant scale for the determination of lipid yields, extraction kinetics, diffusion modeling, and complete lipid composition in term of fatty acids and micronutrients (sterols, tocopherols and tocotrienols). Finally, economic and energetic evaluations of the process were conducted to estimate the cost of manufacturing using 2-methyltetrahydrofuran (MeTHF) as alternative solvent compared to hexane as petroleum solvent.


Subject(s)
Furans/chemistry , Liquid-Liquid Extraction/economics , Plant Oils/isolation & purification , Solvents/chemistry , Fatty Acids, Monounsaturated , Green Chemistry Technology , Hexanes/chemistry , Kinetics , Rapeseed Oil , Solubility
19.
Anal Bioanal Chem ; 407(17): 5189-98, 2015 Jul.
Article in English | MEDLINE | ID: mdl-25749796

ABSTRACT

We report on a new, sensitive, and fast LC-MS/MS method for the simultaneous determination of 25 key sphingolipid components in human plasma, including phosphorylated sphinganine and sphingosine, in a single 9-min run. This method enables an effective and high-throughput coverage of the metabolic changes involving the sphingolipidome during physiological or pathological states. The method is based on liquid-liquid extraction followed by reversed-phase LC-MS/MS. Exogenous odd-chain lipids are used as cost-effective but reliable internal standards. The method was fully validated in surrogate matrix and naive human plasma following FDA guidelines. Sample stability and dilution integrity were also tested and verified.


Subject(s)
Chromatography, High Pressure Liquid/methods , Phospholipids/blood , Sphingolipids/blood , Tandem Mass Spectrometry/methods , Chromatography, High Pressure Liquid/economics , Chromatography, Reverse-Phase/economics , Chromatography, Reverse-Phase/methods , Female , Humans , Limit of Detection , Liquid-Liquid Extraction/economics , Liquid-Liquid Extraction/methods , Male , Reproducibility of Results , Tandem Mass Spectrometry/economics
20.
Anal Chim Acta ; 797: 50-6, 2013 Oct 03.
Article in English | MEDLINE | ID: mdl-24050669

ABSTRACT

A glass liquid-liquid extraction (LLE) microchip with three parallel 3.5 cm long and 100 µm wide interconnecting channels was optimized in terms of more environmentally friendly (greener) solvents and extraction efficiency. In addition, the optimized chip was successfully hyphenated with nano-liquid chromatography with ultraviolet and mass spectrometric detection (nanoLC-UV-MS) for on-line analysis. In this system, sample pretreatment, separation and detection are integrated, which significantly shortens the analysis time, saves labor and drastically reduces solvent consumption. Strychnine was used as model analyte to determine the extraction efficiency of the optimized 3-phase chip. Influence of organic solvent, pH of feed phase, type of alkaloid, and flow rates were investigated. The results demonstrated that the 3-phase chip nanoLC-UV/MS hyphenation combines rapid (~25 s) and efficient (extraction efficiency >90%) sample prep, with automated alkaloid analyses. The method was applied to real samples including Strychnos nux-vomica seeds, Cephaelis ipecacuanha roots, Atropa belladonna leaves, and Vinca minor leaves.


Subject(s)
Alkaloids/isolation & purification , Chromatography, High Pressure Liquid/instrumentation , Liquid-Liquid Extraction/instrumentation , Microfluidic Analytical Techniques/instrumentation , Plants/chemistry , Acetates/chemistry , Chromatography, High Pressure Liquid/economics , Equipment Design , Green Chemistry Technology/economics , Green Chemistry Technology/instrumentation , Liquid-Liquid Extraction/economics , Microfluidic Analytical Techniques/economics , Solvents/chemistry
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