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Ion Mobility Spectrometers as Chromatographic DetectorsInterest in connecting ion mobility spectrometry (IMS) to GC and especially to LC is now growing. One favorable property of IMS is that it can work with ambient pressure and can be easily connected to a gas or liquid chromatograph. Analytical applications of GC–MS and LC–MS are very different and encompass investigations into food, medical science, environment, drugs of abuse, chemical warfare agents, and explosives.
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Comparison of LC–MS and GC–MS for the Analysis of Pharmaceuticals and Personal Care Products in Surface Water and Treated WastewatersWater samples were obtained from the Tar River and a local water treatment plant in eastern North Carolina in spring 2013 and fall 2015 to monitor the presence of a panel of pharmaceutical and personal care products (PPCPs). Samples were extracted by solid phase extraction (SPE) or liquid-liquid extraction and analyzed for parent PPCPs and their metabolites by liquid chromatography-time of flight mass spectrometry (HPLC-TOFMS) and gas chromatography-mass spectrometry (GC-MS). Both extraction and detection methods were compared by their recoveries and detection limits for each compound. Many parent PPCPs and their metabolites were detected including: carbamazepine, iminostillbene, oxcarbazepine, epiandrosterone, loratadine, β-estradiol, triclosan, and others. Liquid-liquid extraction was found to give overall superior recoveries. Furthermore, HPLC-TOFMS gave lower detection limits than GC-MS. Library searching of additional peaks identified further compounds with biological activity. Additionally, the effectiveness of the treatment plant on the removal of the compounds of interest is discussed.
Latest:
Comparison of LC–MS and GC–MS for the Analysis of Pharmaceuticals and Personal Care Products in Surface Water and Treated WastewatersWater samples were obtained from the Tar River and a local water treatment plant in eastern North Carolina in spring 2013 and fall 2015 to monitor the presence of a panel of pharmaceutical and personal care products (PPCPs). Samples were extracted by solid phase extraction (SPE) or liquid-liquid extraction and analyzed for parent PPCPs and their metabolites by liquid chromatography-time of flight mass spectrometry (HPLC-TOFMS) and gas chromatography-mass spectrometry (GC-MS). Both extraction and detection methods were compared by their recoveries and detection limits for each compound. Many parent PPCPs and their metabolites were detected including: carbamazepine, iminostillbene, oxcarbazepine, epiandrosterone, loratadine, β-estradiol, triclosan, and others. Liquid-liquid extraction was found to give overall superior recoveries. Furthermore, HPLC-TOFMS gave lower detection limits than GC-MS. Library searching of additional peaks identified further compounds with biological activity. Additionally, the effectiveness of the treatment plant on the removal of the compounds of interest is discussed.
Latest:
Comparison of LC–MS and GC–MS for the Analysis of Pharmaceuticals and Personal Care Products in Surface Water and Treated WastewatersWater samples were obtained from the Tar River and a local water treatment plant in eastern North Carolina in spring 2013 and fall 2015 to monitor the presence of a panel of pharmaceutical and personal care products (PPCPs). Samples were extracted by solid phase extraction (SPE) or liquid-liquid extraction and analyzed for parent PPCPs and their metabolites by liquid chromatography-time of flight mass spectrometry (HPLC-TOFMS) and gas chromatography-mass spectrometry (GC-MS). Both extraction and detection methods were compared by their recoveries and detection limits for each compound. Many parent PPCPs and their metabolites were detected including: carbamazepine, iminostillbene, oxcarbazepine, epiandrosterone, loratadine, β-estradiol, triclosan, and others. Liquid-liquid extraction was found to give overall superior recoveries. Furthermore, HPLC-TOFMS gave lower detection limits than GC-MS. Library searching of additional peaks identified further compounds with biological activity. Additionally, the effectiveness of the treatment plant on the removal of the compounds of interest is discussed.
Latest:
Comparison of LC–MS and GC–MS for the Analysis of Pharmaceuticals and Personal Care Products in Surface Water and Treated WastewatersWater samples were obtained from the Tar River and a local water treatment plant in eastern North Carolina in spring 2013 and fall 2015 to monitor the presence of a panel of pharmaceutical and personal care products (PPCPs). Samples were extracted by solid phase extraction (SPE) or liquid-liquid extraction and analyzed for parent PPCPs and their metabolites by liquid chromatography-time of flight mass spectrometry (HPLC-TOFMS) and gas chromatography-mass spectrometry (GC-MS). Both extraction and detection methods were compared by their recoveries and detection limits for each compound. Many parent PPCPs and their metabolites were detected including: carbamazepine, iminostillbene, oxcarbazepine, epiandrosterone, loratadine, β-estradiol, triclosan, and others. Liquid-liquid extraction was found to give overall superior recoveries. Furthermore, HPLC-TOFMS gave lower detection limits than GC-MS. Library searching of additional peaks identified further compounds with biological activity. Additionally, the effectiveness of the treatment plant on the removal of the compounds of interest is discussed.
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Simultaneous Quantitation of Buprenorphine and Its Metabolites Using LC–MSAn LC-MS method has been developed for simultaneous quantification of buprenorphine and its three metabolites, namely norbuprenorphine, buprenorphine glucuronide, and norbuprenorphine glucuronide Chromatographic separation was achieved on a C18 column with a gradient of acetonitrile and ammonium acetate buffer (25 mM, pH 6.6). The method run time was 7.5 min. Quantification was performed by selected ion monitoring of [M+H]+ ions of norbuprenorphine glucuronide (590), norbuprenorphine (414), buprenorphine glucuronide (644) and buprenorphine (468). Naloxone (328) (328ng/mL) was used as an internal standard. The samples were processed by protein precipitation and extraction recovery was ≥95% with minimal observed matrix effects (
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Simultaneous Quantitation of Buprenorphine and Its Metabolites Using LC–MSAn LC-MS method has been developed for simultaneous quantification of buprenorphine and its three metabolites, namely norbuprenorphine, buprenorphine glucuronide, and norbuprenorphine glucuronide Chromatographic separation was achieved on a C18 column with a gradient of acetonitrile and ammonium acetate buffer (25 mM, pH 6.6). The method run time was 7.5 min. Quantification was performed by selected ion monitoring of [M+H]+ ions of norbuprenorphine glucuronide (590), norbuprenorphine (414), buprenorphine glucuronide (644) and buprenorphine (468). Naloxone (328) (328ng/mL) was used as an internal standard. The samples were processed by protein precipitation and extraction recovery was ≥95% with minimal observed matrix effects (
Latest:
Simultaneous Quantitation of Buprenorphine and Its Metabolites Using LC–MSAn LC-MS method has been developed for simultaneous quantification of buprenorphine and its three metabolites, namely norbuprenorphine, buprenorphine glucuronide, and norbuprenorphine glucuronide Chromatographic separation was achieved on a C18 column with a gradient of acetonitrile and ammonium acetate buffer (25 mM, pH 6.6). The method run time was 7.5 min. Quantification was performed by selected ion monitoring of [M+H]+ ions of norbuprenorphine glucuronide (590), norbuprenorphine (414), buprenorphine glucuronide (644) and buprenorphine (468). Naloxone (328) (328ng/mL) was used as an internal standard. The samples were processed by protein precipitation and extraction recovery was ≥95% with minimal observed matrix effects (
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Sensitive, Rapid Estimation of Moxidectin in Cattle Hair by LC–MS-MSMoxidectin formulations help to reduce hair loss and irritation due to parasite worms in animals. So Estimation of Moxidectin in hair is important to evaluate therapeutic levels, distribution & accumulation, however estimation is also useful to evaluate harm to birds when they eat animal hair. Hence Moxidectin estimation is required for pharmacokinetic as well as environmental exposure study. Objective of the present work is to develop a rapid, selective method for the estimation of Moxidectin in Cattle Hair by LC-MS/MS. Oxcarbazepine used as a internal standard. Moxidectin extracted from cattle hair by liquid-liquid extraction using Sorenson’s Buffer as digestion solvent for incubation & methyl tert-butyl ether as an extraction solvent. Detection was performed over the range 0.026 to 1.000 ng/mG using MRM in positive polarity at unit resolution under turbo ion spray whereas separation was achieved on Kinetex 100 x 4.6 mm, 5u EVO C18 100A column with Methanol : 10mM Amonium formate pumped as gradient flow with 4.50min run time. Q1 is 640.45 whereas Q3 is sum of 528.50 and 498.50. Validation parameters shown reliable results. Method is applied for the estimation of Moxidectin in cattle Hair.
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The Applicability of Field-Portable GC–MS for the Rapid Sampling and Measurement of High-Boiling-Point Semivolatile Organic Compounds in Environmental SamplesIn this study we report on the use of a field-portable GC-MS with rapid sampling techniques such as solid-phase micro extraction, purge-and-trap, thermal desorption, and heated headspace to provide a fast response for in-field-SVOCs analyses for a wide variety of environmental-type samples including potable waters, tea, plants and road gravel. We will show that this field-portable approach can provide the required sensitivity, selectivity for the effective analysis of SVOCs with very high boiling points such as polycyclic aromatic hydrocarbon (PAHs), pesticides, phenolic compounds and phthalate esters in a number of different field-based samples, in less than 10 minutes.
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Implementation of MicroNIR PAT for Blend MonitoringA wireless NIR spectrometer is deployed on solid dose blending formulation for end-point monitoring. The MicroNIR PAT is democratizing the use NIR spectroscopy in pharmaceutical manufacturing facilitating Quality by Design (QbD) adoption.
Latest:
Sensitive, Rapid Estimation of Moxidectin in Cattle Hair by LC–MS-MSMoxidectin formulations help to reduce hair loss and irritation due to parasite worms in animals. So Estimation of Moxidectin in hair is important to evaluate therapeutic levels, distribution & accumulation, however estimation is also useful to evaluate harm to birds when they eat animal hair. Hence Moxidectin estimation is required for pharmacokinetic as well as environmental exposure study. Objective of the present work is to develop a rapid, selective method for the estimation of Moxidectin in Cattle Hair by LC-MS/MS. Oxcarbazepine used as a internal standard. Moxidectin extracted from cattle hair by liquid-liquid extraction using Sorenson’s Buffer as digestion solvent for incubation & methyl tert-butyl ether as an extraction solvent. Detection was performed over the range 0.026 to 1.000 ng/mG using MRM in positive polarity at unit resolution under turbo ion spray whereas separation was achieved on Kinetex 100 x 4.6 mm, 5u EVO C18 100A column with Methanol : 10mM Amonium formate pumped as gradient flow with 4.50min run time. Q1 is 640.45 whereas Q3 is sum of 528.50 and 498.50. Validation parameters shown reliable results. Method is applied for the estimation of Moxidectin in cattle Hair.
Latest:
The Applicability of Field-Portable GC–MS for the Rapid Sampling and Measurement of High-Boiling-Point Semivolatile Organic Compounds in Environmental SamplesIn this study we report on the use of a field-portable GC-MS with rapid sampling techniques such as solid-phase micro extraction, purge-and-trap, thermal desorption, and heated headspace to provide a fast response for in-field-SVOCs analyses for a wide variety of environmental-type samples including potable waters, tea, plants and road gravel. We will show that this field-portable approach can provide the required sensitivity, selectivity for the effective analysis of SVOCs with very high boiling points such as polycyclic aromatic hydrocarbon (PAHs), pesticides, phenolic compounds and phthalate esters in a number of different field-based samples, in less than 10 minutes.
Latest:
Sensitive, Rapid Estimation of Moxidectin in Cattle Hair by LC–MS-MSMoxidectin formulations help to reduce hair loss and irritation due to parasite worms in animals. So Estimation of Moxidectin in hair is important to evaluate therapeutic levels, distribution & accumulation, however estimation is also useful to evaluate harm to birds when they eat animal hair. Hence Moxidectin estimation is required for pharmacokinetic as well as environmental exposure study. Objective of the present work is to develop a rapid, selective method for the estimation of Moxidectin in Cattle Hair by LC-MS/MS. Oxcarbazepine used as a internal standard. Moxidectin extracted from cattle hair by liquid-liquid extraction using Sorenson’s Buffer as digestion solvent for incubation & methyl tert-butyl ether as an extraction solvent. Detection was performed over the range 0.026 to 1.000 ng/mG using MRM in positive polarity at unit resolution under turbo ion spray whereas separation was achieved on Kinetex 100 x 4.6 mm, 5u EVO C18 100A column with Methanol : 10mM Amonium formate pumped as gradient flow with 4.50min run time. Q1 is 640.45 whereas Q3 is sum of 528.50 and 498.50. Validation parameters shown reliable results. Method is applied for the estimation of Moxidectin in cattle Hair.
Latest:
The Applicability of Field-Portable GC–MS for the Rapid Sampling and Measurement of High-Boiling-Point Semivolatile Organic Compounds in Environmental SamplesIn this study we report on the use of a field-portable GC-MS with rapid sampling techniques such as solid-phase micro extraction, purge-and-trap, thermal desorption, and heated headspace to provide a fast response for in-field-SVOCs analyses for a wide variety of environmental-type samples including potable waters, tea, plants and road gravel. We will show that this field-portable approach can provide the required sensitivity, selectivity for the effective analysis of SVOCs with very high boiling points such as polycyclic aromatic hydrocarbon (PAHs), pesticides, phenolic compounds and phthalate esters in a number of different field-based samples, in less than 10 minutes.
Latest:
Sensitive, Rapid Estimation of Moxidectin in Cattle Hair by LC–MS-MSMoxidectin formulations help to reduce hair loss and irritation due to parasite worms in animals. So Estimation of Moxidectin in hair is important to evaluate therapeutic levels, distribution & accumulation, however estimation is also useful to evaluate harm to birds when they eat animal hair. Hence Moxidectin estimation is required for pharmacokinetic as well as environmental exposure study. Objective of the present work is to develop a rapid, selective method for the estimation of Moxidectin in Cattle Hair by LC-MS/MS. Oxcarbazepine used as a internal standard. Moxidectin extracted from cattle hair by liquid-liquid extraction using Sorenson’s Buffer as digestion solvent for incubation & methyl tert-butyl ether as an extraction solvent. Detection was performed over the range 0.026 to 1.000 ng/mG using MRM in positive polarity at unit resolution under turbo ion spray whereas separation was achieved on Kinetex 100 x 4.6 mm, 5u EVO C18 100A column with Methanol : 10mM Amonium formate pumped as gradient flow with 4.50min run time. Q1 is 640.45 whereas Q3 is sum of 528.50 and 498.50. Validation parameters shown reliable results. Method is applied for the estimation of Moxidectin in cattle Hair.
Latest:
Implementation of MicroNIR PAT for Blend MonitoringA wireless NIR spectrometer is deployed on solid dose blending formulation for end-point monitoring. The MicroNIR PAT is democratizing the use NIR spectroscopy in pharmaceutical manufacturing facilitating Quality by Design (QbD) adoption.
Latest:
Advanced Structural Mass Spectrometry for Systems Biology: Pulling the Needles from HaystacksIon mobility–mass spectrometry (IM-MS) is outlined as a separations method, several examples of the utility of IM-MS for complex biological measurements are illustrated, and the implications of this approach for systems biology research are discussed.
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Agilent MicroLab Software with Spectroscopy Configuration Manager and Spectroscopy Database Administrator (SCM/SDA)This technical note describes features and functionality of Agilent MicroLab software (version 5.2 and later) in combination with SCM and SDA for data management and electronic traceability, which enable customers to implement the guidelines of 21 CFR Part 11.
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Agilent Cary 630 FTIR Spectrometer Quickly Identifies and Qualifies PharmaceuticalsThis application note describes a very sensitive classification method, partial least squares–discriminant analysis (PLS-DA), incorporated in Agilent innovative MicroLab software, to classify and qualify materials of interest with greater sensitivity and specificity than possible with simple library search methods.
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Enhancing Confidence in ComplianceThis note highlights OpenLAB ECM Compliance Pack for UV-Vis Benefits such as efficient data storage and retrieval, security, data integrity and traceability, and 21 CFR Part II Comliance.
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Optimization of ED-XRF Excitation Configuration Parameters to Determine Trace-Element Concentrations in Organic and Inorganic Sample MatricesThis month’s column will describe a novel ED-XRF system, which utilizes a combination of a Bragg polarizer, used simultaneously with a direct excitation source, together with a novel, highly annealed pyrolytic graphite (HAPG) crystal as a band-pass filter. By selection of the optimum configuration, it will allow for high precision of minor and major elements across a wide wavelength range and/or lower detection capability for smaller groups of elements from potassium to manganese. To show the practical benefits of this technology, this study will focus on these performance metrics for the determination of titanium in polymer samples, together with the multielement analysis of high purity graphite using the ashing sample preparation method. In particular, it will be shown that the improved performance for graphite will allow for lower sample weights to be used resulting in significantly shorter ashing times, which is a requirement for high sample workload laboratories and process control applications.
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Analysis of the Brill Transition and Reversible Brill Transition in Nylon 6,6 by Raman SpectroscopyThis article verified the Brill transition in nylon 6,6 by Raman spectroscopy through heating and cooling processes of the sample. When nylon is heated at around 160 C a crystalline phase transition occurs from a triclinic structure at room temperature to a pseudohexagonal structure above that temperature. This phase transition is known as the Brill Transition. With temperature-dependent Raman scattering measurements, it was possible to determine the vibrational behavior of nylon 6,6 during the Brill transition, and consequently to identify the main Raman bands associated with the Brill transition.
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Analysis of the Brill Transition and Reversible Brill Transition in Nylon 6,6 by Raman SpectroscopyThis article verified the Brill transition in nylon 6,6 by Raman spectroscopy through heating and cooling processes of the sample. When nylon is heated at around 160 C a crystalline phase transition occurs from a triclinic structure at room temperature to a pseudohexagonal structure above that temperature. This phase transition is known as the Brill Transition. With temperature-dependent Raman scattering measurements, it was possible to determine the vibrational behavior of nylon 6,6 during the Brill transition, and consequently to identify the main Raman bands associated with the Brill transition.
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US EPA SW-846 Method 6010C Using the Prodigy7 High-Dispersion ICP IntroductionThis application note describes the capability of the Teledyne Leeman Lab's Prodigy7 High-Dispersion ICP for performing analysis according to SW-846 Method 6010C.
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Probing Aqueous Surfaces by TOF-SIMSA breakthrough using a microfluidic interface to conduct sensitive time-of-flight secondary ion mass spectrometry (TOF-SIMS) analysis and study liquid surfaces in situ under vacuum conditions is described here.
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Non-invasive Combustion DiagnosticsPLIF, PIV and next generation imaging detectors - Combustion processes, if uncontrolled, are inherently inefficient and increasing the efficiency of combustion in engines, gas burners and furnaces is a significant challenge for the future due to limited fossil fuel resources and their effects on the environment.
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Non-invasive Combustion DiagnosticsPLIF, PIV and next generation imaging detectors - Combustion processes, if uncontrolled, are inherently inefficient and increasing the efficiency of combustion in engines, gas burners and furnaces is a significant challenge for the future due to limited fossil fuel resources and their effects on the environment.
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Determination of Very Low Abundance Diagnostic Proteins in Serum Using Immunocapture LC–MS/MSThere is growing interest in the determination of endogenous proteins in biological samples for diagnostic purposes, because a concentration increase or decrease of such proteins can allows us to monitor the state of a pathological condition such as cancer. Immunocapture LC–MS/MS analysis combines the workflow of conventional immunological assays with LC–MS analysis. This article describes typical challenges, such as cross reactivity and the mass spectrometer’s dynamic range, as well as the advantages of isoform differentiation and multiplexing.
