Beizhan Yan, Masha Pitiranggon, James Ross, Thomas Arthen-Engeland, Andreas Stelter, Steven N Chillrud
{"title":"Validation of Miniaturized Particulate-Matter Real-Time Samplers for Characterizing Personal Polycyclic Aromatic Hydrocarbon Exposure.","authors":"Beizhan Yan, Masha Pitiranggon, James Ross, Thomas Arthen-Engeland, Andreas Stelter, Steven N Chillrud","doi":"10.4172/2155-9872.1000403","DOIUrl":"10.4172/2155-9872.1000403","url":null,"abstract":"<p><p>This study validates the analysis of polycyclic aromatic hydrocarbons (PAHs) in microgram levels of particulate matter (PM) collected on filters by two low-flow rate, real-time monitors, microPEM™ and microAeth<sup>®</sup>. Particle-associated PAHs were analyzed by a coupling of a gas chromatograph to a sensitive, atmospheric-pressure laser ionization-mass spectrometer. Air particulate samples were collected over the course of one or two days in the living room of a fourth-floor apartment in New York City. Three types of samplers, the two aforementioned personal samplers and a high-flow rate pump (4 liters per minute), were operated side by side, and three samples of each type were collected during each sampling period. Intrasampler agreement as measured by relative standard deviation (RSD) was within 1% to 18%. After background subtraction, total PAH measured by all three sampler types had good agreement (R=0.99). This ability to accurately characterize personal PAH exposure in archived filters collected by these real-time samplers could provide additional important PAH exposure information that can benefit many environmental health studies using these monitors.</p>","PeriodicalId":89684,"journal":{"name":"Journal of analytical & bioanalytical techniques","volume":"9 2","pages":""},"PeriodicalIF":0.0,"publicationDate":"2018-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.4172/2155-9872.1000403","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"36308134","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Stuart Farquharson, Kathryn Dana, Chetan Shende, Zachary Gladding, Jenelle Newcomb, Jessica Dascher, Ismene L Petrakis, Albert J Arias
{"title":"Rapid Identification of Buprenorphine in Patient Saliva.","authors":"Stuart Farquharson, Kathryn Dana, Chetan Shende, Zachary Gladding, Jenelle Newcomb, Jessica Dascher, Ismene L Petrakis, Albert J Arias","doi":"10.4172/2155-9872.1000368","DOIUrl":"https://doi.org/10.4172/2155-9872.1000368","url":null,"abstract":"<p><p>Buprenorphine is becoming the medication of choice to help patients withdraw from opioid addiction. However, treatment is compromised by the inability of physicians to assess patient usage during scheduled examinations. Here we describe the development of a point-of-care (POC) analyzer that can rapidly measure both illicit and treatment drugs in patient saliva, ideally in the physician's office, and with a degree of accuracy similar to chromatography. The analyzer employs a relatively simple supported liquid extraction to isolate the drugs from the saliva and surface-enhanced Raman spectroscopy (SERS) to detect the drugs. The SERS-based POC analyzer was used to identify buprenorphine and opioids in saliva samples by matching library spectra to samples collected from 7 veterans. The total analysis time, including sample preparation, was ~25 minutes. Buprenorphine concentration was estimated between 0 and 3 μg/mL. While no other prescription opioids were detected in any samples, heroin was identified in one sample; Δ-9 tetrahydrocannabinol (THC) was detected in 3 samples; and acetaminophen, caffeine, and nicotine were detected in several samples, none of which interfered with the measurements. The analysis was in very good agreement with urinalysis, correctly identifying the presence or absence of buprenorphine and THC in 13 of 14 measurements.</p>","PeriodicalId":89684,"journal":{"name":"Journal of analytical & bioanalytical techniques","volume":"8 3","pages":""},"PeriodicalIF":0.0,"publicationDate":"2017-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.4172/2155-9872.1000368","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"35541970","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Feng Jin, Salil Kumar Bhowmik, Vasanta Putluri, Franklin Gu, Jie Gohlke, Friedrich Carl Von Rundstedt, Subhamoy Dasgupta, Rashmi Krishnapuram, Bert W O'Malley, Arun Sreekumar, Nagireddy Putluri
{"title":"A Novel [<sup>15</sup>N] Glutamine Flux using LC-MS/MS-SRM for Determination of Nucleosides and Nucleobases.","authors":"Feng Jin, Salil Kumar Bhowmik, Vasanta Putluri, Franklin Gu, Jie Gohlke, Friedrich Carl Von Rundstedt, Subhamoy Dasgupta, Rashmi Krishnapuram, Bert W O'Malley, Arun Sreekumar, Nagireddy Putluri","doi":"10.4172/2155-9872.1000267","DOIUrl":"https://doi.org/10.4172/2155-9872.1000267","url":null,"abstract":"<p><p>The growth of cancer cells relies more on increased proliferation and autonomy compared to non-malignant cells. The rate of de novo nucleotide biosynthesis correlates with cell proliferation rates. In part, glutamine is needed to sustain high rates of cellular proliferation as a key nitrogen donor in purine and pyrimidine nucleotide biosynthesis. In addition, glutamine serves as an essential substrate for key enzymes involved in the de novo synthesis of purine and pyrimidine nucleotides. Here, we developed a novel liquid chromatography (LC-MS) to quantify glutamine-derived [15N] nitrogen flux into nucleosides and nucleobases (purines and pyrimidines). For this, DNA from 5637 bladder cancer cell line cultured in 15N labelled glutamine and then enzymatically hydrolyzed by sequential digestion. Subsequently, DNA hydrolysates were separated by LC-MS and Selected Reaction Monitoring (SRM) was employed to identify the nucleobases and nucleosides. Thus, high sensitivity and reproducibility of the method make it a valuable tool to identify the nitrogen flux primarily derived from glutamine and can be further adaptable for high throughput analysis of large set of DNA in a clinical setting.</p>","PeriodicalId":89684,"journal":{"name":"Journal of analytical & bioanalytical techniques","volume":"6 5","pages":""},"PeriodicalIF":0.0,"publicationDate":"2015-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.4172/2155-9872.1000267","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"34371121","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"A Simple and Rapid LC-MS/MS Method for the Determination of BMCL26 a Novel Anti-Parasitic Agent in Rat Plasma","authors":"R. Voggu, Xiang Zhou, Bin Su, B. Guo","doi":"10.4172/2155-9872.1000266","DOIUrl":"https://doi.org/10.4172/2155-9872.1000266","url":null,"abstract":"BMCL26 is a potential drug derived from nimesulide, which has exhibited the substantial anti-parasitic activity in various cell lines. To conduct various pharmacological and toxicological properties of this drug, we developed and validated a rapid LC-MS/MS method for its quantification in accordance with the FDA guidelines. Protein precipitation with 0.1% formic acid in acetonitrile was used to extract the analytes along with the internal standard (JCC76) from rat plasma. It was found that the calibration curve of the method had an excellent linearity (r2 ≥ 0.9993) for the analyte concentration ranging from 0.5 to 100 ng/mL with acceptable inter- and intra-assay, precision, accuracy and stability. The matrix effect and extraction recovery were in the range of 101.30–110.10% and 90.16– 105.00%, respectively. This LC-MS/MS method is simple and rapid and can be used in the future pharmaceutical studies of BMCL26.","PeriodicalId":89684,"journal":{"name":"Journal of analytical & bioanalytical techniques","volume":"6 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2015-08-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.4172/2155-9872.1000266","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"70323168","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Kathryn Dana, Chetan Shende, Hermes Huang, Stuart Farquharson
{"title":"Rapid Analysis of Cocaine in Saliva by Surface-Enhanced Raman Spectroscopy.","authors":"Kathryn Dana, Chetan Shende, Hermes Huang, Stuart Farquharson","doi":"10.4172/2155-9872.1000289","DOIUrl":"10.4172/2155-9872.1000289","url":null,"abstract":"<p><p>Increases in illicit drug use and the number of emergency-room visits attributable to drug misuse or abuse highlight the need for an efficient, reliable method to detect drugs in patients in order to provide rapid and appropriate care. A surface-enhanced Raman spectroscopy (SERS)-based method was successfully developed to rapidly measure cocaine in saliva at clinical concentrations, as low as 25 ng/mL. Pretreatment steps comprising chemical separation, physical separation, and solid-phase extraction were investigated to recover the analyte drug from the saliva matrix. Samples were analyzed using Fourier-transform (FT) and dispersive Raman systems, and statistical analysis of the results shows that the method is both reliable and accurate, and could be used to quantify unknown samples. The procedure requires minimal space and equipment and can be completed in less than 16 minutes. Finally, due to the inclusion of a buffer solution and the use of multiple robust pretreatment steps, with minimal further development this method could also be applied to other drugs of interest.</p>","PeriodicalId":89684,"journal":{"name":"Journal of analytical & bioanalytical techniques","volume":"6 1","pages":"1-5"},"PeriodicalIF":0.0,"publicationDate":"2015-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC4725314/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"70323370","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Albert N Ngo, Miezan Jm Ezoulin, Ibrahima Youm, Bi-Botti C Youan
{"title":"Optimal Concentration of 2,2,2-Trichloroacetic Acid for Protein Precipitation Based on Response Surface Methodology.","authors":"Albert N Ngo, Miezan Jm Ezoulin, Ibrahima Youm, Bi-Botti C Youan","doi":"10.4172/2155-9872.1000198","DOIUrl":"https://doi.org/10.4172/2155-9872.1000198","url":null,"abstract":"<p><p>For low protein concentrations containing biological samples (in proteomics) and for non proteinaceous compound assays (in bioanalysis), there is a critical need for a simple, fast, and cost-effective protein enrichment or precipitation method. However, 2,2,2-trichloroacetic acid (TCA) is traditionally used for protein precipitation at ineffective concentrations for very low protein containing samples. It is hypothesized that response surface methodology, can be used to systematically identify the optimal TCA concentration for protein precipitation in a wider concentration range. To test this hypothesis, a central composite design is used to assess the effects of two factors (X<sub>1</sub> = volume of aqueous solution of protein, and X<sub>2</sub> = volume of TCA solution 6.1N) on the optical absorbance of the supernatant (Y<sub>1</sub>), and the percentage of protein precipitated (Y<sub>2</sub>). Using either bovine serum albumin (BSA) as a model protein or human urine (with 20 ppm protein content), 4% w/v (a saddle point) is the optimal concentration of the TCA solution for protein precipitation that is visualized by SDS-PAGE analysis. At this optimal concentration, the Y<sub>2</sub>-values range from 76.26 to 92.67% w/w for 0.016 to 2 mg/mL of BSA solution. It is also useful for protein enrichment and xenobiotic analysis in protein-free supernatant as applied to tenofovir (a model HIV microbicide). In these conditions, the limit of detection and limit of quantitation of tenofovir are respectively 0.0014 mg/mL and 0.0042 mg/mL. This optimal concentration of TCA provides optimal condition for protein purification and analysis of any xenobiotic compound like tenofovir.</p>","PeriodicalId":89684,"journal":{"name":"Journal of analytical & bioanalytical techniques","volume":"5 4","pages":""},"PeriodicalIF":0.0,"publicationDate":"2014-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.4172/2155-9872.1000198","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"33112713","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Shunji Tomatsu, Tsutomu Shimada, Robert W Mason, Joan Kelly, William A LaMarr, Eriko Yasuda, Yuniko Shibata, Hideyuki Futatsumori, Adriana M Montaño, Seiji Yamaguchi, Yasuyuki Suzuki, Tadao Orii
{"title":"Assay for Glycosaminoglycans by Tandem Mass Spectrometry and its Applications.","authors":"Shunji Tomatsu, Tsutomu Shimada, Robert W Mason, Joan Kelly, William A LaMarr, Eriko Yasuda, Yuniko Shibata, Hideyuki Futatsumori, Adriana M Montaño, Seiji Yamaguchi, Yasuyuki Suzuki, Tadao Orii","doi":"10.4172/2155-9872.S2-006","DOIUrl":"https://doi.org/10.4172/2155-9872.S2-006","url":null,"abstract":"<p><p>Glycosaminoglycans (GAGs) are distributed in the whole body and play a variety of important physiological roles associated with inflammation, growth, coagulation, fibrinolysis, lipolysis, and cell-matrix biology. Accumulation of undegraded GAGs in lysosomes gives rise to a distinct clinical syndrome, mucopolysaccharidoses. Measurement of each specific GAG in a variety of specimens is urgently required to understand GAG interaction with other molecules, physiological status of patients, and prognosis and pathogenesis of the disease. We established a highly sensitive and accurate tandem mass spectrometry (LC-MS/MS) method for measurements of disaccharides derived from four specific GAGs [dermatan sulfate (DS), heparan sulfate (HS), keratan sulfate (KS), and chondroitin sulfate (CS)]. Disaccharides were produced by specific enzyme digestion of each GAG, and quantified by negative ion mode of multiple reaction monitoring. Subclasses of HS and GAGs with identical molecular weights can be separated using a Hypercarbcolumn (2.0 mm×50 mm, 5 μm) with an aectonitrile gradient in ammonium acetate (pH 11.0). We also developed a GAG assay by RapidFire with tandem mass spectrometry (RF-MS/MS). The RF system consists of an integrated solid phase extraction robot that binds and de-salts samples from assay plates and directly injects them into a MS/MS detector, reducing sample processing time to ten seconds. RF-MS/MS consequently yields much faster throughput than conventional LC-MS/MS-based methods. However, the RF system does not have a chromatographic step, and therefore, cannot distinguish GAGs that have identical molecular weights. Both methods can be applied to analysis of dried blood spots, blood, and urine specimens. In this article, we compare the assay methods for GAGs and describe their potential applications.</p>","PeriodicalId":89684,"journal":{"name":"Journal of analytical & bioanalytical techniques","volume":"2014 Suppl 2","pages":"006"},"PeriodicalIF":0.0,"publicationDate":"2014-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.4172/2155-9872.S2-006","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"32539646","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Vivek Agrahari, Jianing Meng, Tao Zhang, Bi-Botti C Youan
{"title":"Application of Design of Experiment and Simulation Methods to Liquid Chromatography Analysis of Topical HIV Microbicides Stampidine and HI443.","authors":"Vivek Agrahari, Jianing Meng, Tao Zhang, Bi-Botti C Youan","doi":"10.4172/2155-9872.1000180","DOIUrl":"https://doi.org/10.4172/2155-9872.1000180","url":null,"abstract":"<p><p>This study intended to determine if experimental design and Monte Carlo simulation methods can be utilized to optimize the liquid chromatography (LC) analysis of active molecules. The method was applied for the simultaneous analysis of two topical microbicides, stampidine (STP) and HI443 in bulk and nanoformulations. The Plackett-Burman design was used for screening; whereas, Box-Behnken design was used to evaluate the main and interaction effects of the selected factors on the responses, namely peak area of STP (Y<sub>1</sub>), HI443 (Y<sub>2</sub>), tailing of STP (Y<sub>3</sub>), and HI443 (Y<sub>4</sub>). The Monte Carlo simulation was applied to get the minimum defect rate (DR) of the process. The optimized LC conditions were found to be X<sub>1</sub>; flow rate: 0.6 mL/min, X<sub>2</sub>; injection volume: 18 μL, and X<sub>3</sub>; initial gradient acetonitrile ratio: 92% v/v with a minimal DR of 0.077%. The optimized method was applied to determine the percent encapsulation efficiency (%EE) and <i>in vitro</i> release profile of STP and HI443 from solid lipid nanoparticles (SLNs). The %EE of STP and HI443 in SLNs was found to be 30.56 ± 9.44 and 94.80 ± 21.90% w/w, respectively, (n=3). It was observed that the release kinetics of STP followed the first order, whereas, HI443 followed the Peppas kinetic model in SLNs. The LC method was also applied for the estimation of molar extinction coefficients (<i>ε<sub>270</sub></i> ) of both drugs for the first time. These values were estimated to be 7,569.03 ± 217.96 and 17,823.67 ± 88.12 L/mol/cm for STP and HI443, respectively, (n=3). The results suggest that experimental design and Monte Carlo simulation can be effectively used to reduce the DR of a process and to optimize the chromatographic conditions for the analysis of bio-active agents as applied in this study.</p>","PeriodicalId":89684,"journal":{"name":"Journal of analytical & bioanalytical techniques","volume":"5 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2014-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.4172/2155-9872.1000180","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"33127322","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Thallapuranam K Suresh Kumar, Ryan Thurman, Srinivas Jayanthi
{"title":"In-Cell NMR Spectroscopy-<i>In vivo</i> Monitoring of the Structure, Dynamics, Folding, and Interactions of Proteins at Atomic Resolution.","authors":"Thallapuranam K Suresh Kumar, Ryan Thurman, Srinivas Jayanthi","doi":"10.4172/2155-9872.1000e112","DOIUrl":"https://doi.org/10.4172/2155-9872.1000e112","url":null,"abstract":"","PeriodicalId":89684,"journal":{"name":"Journal of analytical & bioanalytical techniques","volume":"4 1","pages":"e112"},"PeriodicalIF":0.0,"publicationDate":"2013-01-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC3744243/pdf/nihms-454212.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"31666769","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Alejandro A Pezzulo, Muhammad H Asif, Magnus Willander, Joseph Zabner
{"title":"In Situ Quantification of Glucose Concentration in Airway Surface Liquid With Functionalized ZnO Nanorod-Coated Microelectrodes.","authors":"Alejandro A Pezzulo, Muhammad H Asif, Magnus Willander, Joseph Zabner","doi":"10.4172/2155-9872.S7-002","DOIUrl":"10.4172/2155-9872.S7-002","url":null,"abstract":"<p><p>The surface of the airways that conduct gases into and out of the lungs has components that protect the host from inhaled and aspirated pathogens. The thin (4-7 µm height) layer of airway surface liquid (ASL) that lines the airways has physicochemical properties that are important for normal function of these antimicrobial components. Among these properties, low glucose concentration is required for normal antimicrobial activity. Current methods for assessing the ASL have important flaws (temporal resolution, dilution factors, collection volume), which have been a recurring obstacle for understanding diseases in which ASL composition is abnormal. To circumvent these problems, microelectrodes coated with ZnO nanorods and immobilized glucose oxidase was used to determine glucose concentration in ASL of well-differentiated cultures of human airway epithelia. The sensor responded to glucose linearly over a concentration range of 0.128 to 8 mM and the effects of electroactive interferents were minimal. The measured concentration of glucose in ASL was consistent with values previously reported. This method confirms the presence of a transepithelial glucose concentration gradient in human airway epithelia and is an important step towards characterizing the physicochemical properties of ASL and understanding diseases caused by changes in ASL composition.</p>","PeriodicalId":89684,"journal":{"name":"Journal of analytical & bioanalytical techniques","volume":"S7 2","pages":""},"PeriodicalIF":0.0,"publicationDate":"2011-08-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC3514975/pdf/nihms333944.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"31111928","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}