Abstract: Disclosed are LC-LC-MS/MS techniques for the analysis of endogenous peptides and other highly polar small molecules. The methods and systems of the present invention can be applied in all industries that utilize LC-MS/MS for the evaluation and quantification of biological analytes in complex matrixes.

Abstract: A sample injection apparatus and a liquid chromatography apparatus including the sample injection apparatus are provided. The sample injection apparatus includes a sampling vessel into which a sample is supplied, a sampling needle for aspirating and ejecting the sample, a cleaning part into which a cleaning liquid for cleaning at least the sampling needle is supplied, a sample injection part for injecting the sample ejected from the sampling needle into a moving liquid, and a needle transfer part for transferring the sampling needle among the sampling vessel, the cleaning part and the sample injection part, wherein the cleaning part includes an ultrasonic vibrator for generating an ultrasonic wave in the cleaning liquid.

Abstract: A carbon monolith includes a robust carbon monolith characterized by a skeleton size of at least 100 nm, and a hierarchical pore structure having macropores and mesopores.

Abstract: The invention provides methods for analysing heparins, low-molecular-weight heparins, ultralow-molecular-weight heparins, and oligosaccharides by high performance liquid chromatography a stationary phase dynamically coated with a quaternary ammonium salt. The methods of the invention may be used to analyse samples without pre-treatment or to analyse samples that have been partially or exhaustively depolymerised and, optionally, reduced. Specific saccharides can be detected.

Abstract: The present invention provides a novel method for assaying OPC contained in natural substances, foods and beverages, pharmaceuticals and/or cosmetics. The present invention is a novel method for assay of OPC which assays anthocyanidin, obtained by hydrolysis of OPC, to determine the total amount of OPC, and elucidates the proportions of the polymerization degrees of OPC by high performance liquid chromatography (HPLC) to determine the contents of the respective polymers in OPC.

Abstract: The present invention provides a method for determining a level of a RuBP, PGA, 2-PA in a photosynthetic cellular extract by resolving at least one RuBP, PGA, or 2-PA or combinations thereof in a photosynthetic cellular extract obtained from a plant. In another aspect, it provides for detecting at least one resolved RuBP, PGA, or 2-PA or combinations, thereby determining a level of the resolved RuBP, PGA, or 2-PA or combinations. In one aspect the photosynthetic cellular extract is obtained from a plant subjected to an abiotic stress. A method of the invention can be useful, for example, for identifying plants with increased photosynthetic performance. Also included herein is a high throughput system for identifying a plant with increased photosynthetic performance.

Abstract: An object of the present invention is to provide a process according to which 5-ene-3-one or 3,6-dione derivatives of sterols can be synthesized with a better yield, as well as a process for production of lipid metabolism improvers, foods, drinks, and animal feeds containing the 5-ene-3-one or 3,6-dione derivatives of sterols. The process for production of 5-ene-3-one or 3,6-dione derivatives of sterols of the present invention involves preparing a culturing solution containing an Arthrobacter bacterium, which is a microorganism exhibiting a cholesterol oxidase activity, and then, adding to the culturing solution an equivalent amount of hexane so as to prepare a bilayer solution consisting of an aqueous layer and a hydrocarbon-based solvent layer. Thereafter, sterol, or a derivative thereof, is made as a substrate contained therein, a reaction performed with cholesterol oxidase at 30° C. for 2 days, and, ethanol then added to separate a hydrocarbon-based solvent layer.

Abstract: The method comprising the steps of engaging the flow circuit of the detector with a reference fluid, accepting a sample in the flow circuit of the detector, sensing an attribute of the sample for determining a characteristic of the sample, changing the direction of the flow of the sample in the flow circuit, and purging the sample from the flow circuit such that the flow circuit is ready to accept another sample. Another method provides the steps of engaging the flow circuit of the detector with a reference fluid, inserting a sample in the flow circuit juxtaposed to the reference fluid, sensing an attribute of the sample for determining a characteristic of the sample, and deviating the direction of the flow of the sample from the flow circuit for purging the sample from the flow circuit such that the reference fluid is maintained in the flow circuit.

Abstract: A device comprising a pressure monitor and a control means that receives a signal representing measured pressure at the pressure monitor and controls the controllable elements of a fluid system is utilized to monitor a fluid system for error conditions, to optimize operations and to diagnose the fluid system. By following a testing protocol that selectively enables parts of the system, the control means narrows the list of possible failing components. Comparing the measured pressure against normal pressures allows the device to identify error conditions. Determining the volume of fluid being transported and controlling the duration of the flow optimizes operation of the fluid system.

Abstract: The invention relates to the analytical determination of poloxamers in a liquid protein sample.

Abstract: A correlation method for measuring total and fractional flow rates of multiphase immiscible media comprises identifying two control sections along the multiphase flow, and scanning each control section so as to measure fluctuations in the dielectric flow characteristics in each section, the scanning signals for each section comprising rotating high-frequency electric and magnetic fields with one common carrier frequency. The received scanning signals are independently processed so as to identify the peak amplitude-frequency and gain-phase characteristics of the signals, and the results of all measurements are used for calculating the correlation functions. The scanning signals generated by the rotating high-frequency electric field are amplified by means of a normalizing scale factor, and all four scanning signals are additionally processed by a microprocessor. Total and factional flow rates are determined by comparing the measured characteristics with reference characteristics stored in a database.

Abstract: The present invention relates to a process for preparing vildagliptin of formula (I) with high chemical and enantiomeric purity and compositions comprising vildagliptin. In addition, the present invention relates to (2S,2?S)-1,1?-[[(3-hydroxytricyclo[3.3.1.13,7]dec-1-yl)imino]bis(1-oxo-2,1-ethanediyl)]di(2-pyrrolidinecarbonitrile) of formula (II), processes for preparing, and compositions comprising a compound for formula (II). Furthermore, the invention relates to processes for determining the purity of vildagliptin using a compound of formula (II).

Abstract: Application of a reference mixture of natural products for systematic analysis and comparison of the properties of biphasic solvent systems in counter-current/partition chromatography. Because the reference mixture is comprised of compounds with varying polarities, functional groups, and structural features it provides a rational method for mapping the optimal resolution polarity range of a particular solvent system. The mapping of optimal resolution polarity ranges of solvent systems provided for the description of the overall optimal resolution polarity range of a solvent system family, comprised of the same solvents in different proportions. By comparing the reference mixture performance in the individual members of a solvent system family, the solvent system that best functions as the representative of, or portal to, the solvent system families is determined. Use of the reference mixture also afforded a method to compare the overall optimal resolution polarity ranges of solvent system families.

Abstract: A method of analysis of lipoproteins according to the present invention comprises the steps of: separating a plurality of classes of lipoproteins contained in a subject sample by liquid chromatography and then detecting signals derived from components included in the separated lipoproteins; and assuming that the lipoproteins are constituted of subclasses estimated from component peaks comprising anchor peaks and extra essential peaks and then calculating an approximated curve corresponding to summation of the component peaks using the above described detected signals.

Abstract: An ultrahigh-pressure dual on-line solid phase extraction/capillary reverse-phase liquid chromatography (DO-SPE/cRPLC) system is provided.

Abstract: The present invention provides apparatus and methods for controlling liquid chromatography flow, while preserving optimum separation of analyte components and providing a longer time for detector analysis to simultaneously increase detection sensitivity and resolution.

Abstract: A method for analyzing a multi-channel chromatogram is realized for accurately resolving overlapping peaks on a multi-channel chromatogram to permit analysis of the composition of a sample. First, components of overlapping peaks are specified. A data matrix Dij is determined, and compressed in the wavelength direction to obtain a data matrix vector Di. Next, the two-dimensional data is deconvoluted, final standard deviation s0 is registered, and the deconvoluted two-dimensional data is reconvoluted to a retention intensity matrix. A quantitative spectral intensity matrix is computed, components are identified, and the identified components are quantified. Subsequently, an eigenvalue problem is solved, and the number n of components is estimated. The deconvolution and computation of the eigenvalue problem are iteratively executed until the peaks are isolated. Then, elution profiles are calculated, the components are identified, and the identified components are quantified.

Abstract: This liquid feeding system has the first and second pumps each of which is provided with a plunger. Liquid sucked through each of the pump suction ports is discharged out of the discharging port through the first pump and/or second pump. Under the starting operation mode, the second pump is stopped and only the first pump is operated. When the discharging pressure at the discharging port reaches up to a predetermined value, the starting operation mode is changed over to the normal operation mode. Under the normal operation mode, the first pump is stopped and only the second pump is operated.

Abstract: A sample injection apparatus and sample injection method capable of sufficiently reducing carry-over, having simple cleaning means for a short cleaning time period, a small influence of vibration of the cleaning means, and a small error in the amount of injected sample and preventing the durability of a sampling needle from being lowered, and a liquid chromatography apparatus having the sample injection apparatus are provided.

Abstract: An improved system, device and method for characterizing a fluid sample that includes injecting a fluid sample into a mobile phase of a flow characterization system, and detecting a property of the fluid sample or of a component thereof with a flow detector comprising a mechanical resonator, preferably one that is operated at a frequency less than about 1 MHz, such as a tuning fork resonator.

Abstract: There is provided a method that includes, (a) monitoring a pressure on a fluid being conveyed through an intake tube into a chamber by a pump, (b) determining a deviation of the pressure from a predefined value, (c) determining a blockage of the intake tube based on the deviation, and (d) determining an amount of an adjustment of a parameter of the pump to compensate for the blockage.

Abstract: A device adapted to hold and compress a granular medium is disclosed. The device includes a body having an opening. A channel is positioned in fluid communication with the opening. A flexible substrate is attached to the body overlying the channel. The substrate and the channel cooperate to form a conduit in fluid communication with the opening. A compression member is mounted on the body. The compression member is engageable with the substrate. Engagement of the substrate by the compression member compresses the granular medium within the conduit. A plug blocks the opening and retains the granular medium within the conduit.

Abstract: The present invention provides a chromatograph/mass spectrometer capable of producing a composite chromatogram from plural chromatogram signals without causing the baseline level to rise or the intensity of the chromatogram peak to decrease. The chromatograph/mass spectrometer includes a chromatograph unit for separating a sample into components in the order of time, a mass spectrometer unit for analyzing the components of the sample, and a signal generator for producing a signal carrying a chromatogram obtained by the analysis. It also includes a chromatogram composer for receiving signals of plural chromatograms simultaneously measured under different conditions, for choosing the largest value of the plural signals for each point in time, and for integrating the chosen values to produce a composite chromatogram.

Abstract: When an instruction by a person in charge is required during an analysis operation, a transmitted e-mail processing unit creates an e-mail that includes, as a message or an attached file, information concerning data to be currently analyzed and an analysis condition, and transmits the e-mail to the e-mail address of the person in charge. The person in charge, at a remote area, employs a locally available PC to read the e-mail, and transmits, to an analysis apparatus, a response e-mail that includes an instruction command. The e-mail is read through a communication controller, and a received case name confirmation unit and a sender verification unit examine the received e-mail to determine whether it is a control e-mail issued by an authorized sender. Thereafter, a command extraction unit extracts a control command from the e-mail. Upon receiving this command, an analysis controller controls the individual sections of an analysis unit.

Abstract: Systems and methods for analyzing a plurality of samples in parallel include a plurality of liquid phase separation regions, a plurality of microfluidic storage regions, and a common mass spectrometer. Samples are separated in parallel in the separation regions to yield a plurality of output streams that are stored in the storage regions. The contents of each storage region, or at least a representative portion thereof, are sequentially discharged, ionized, and directed to the inlet of a mass spectrometer. In this manner, multiple separations are conducted in parallel with outputs provided serially to a common mass spectrometer without any loss of data. Microfluidic storage regions minimize diffusion between bands of separated samples. Portions of separated samples may be directed to fraction collectors.

Abstract: To economically perform preparatory chromatography, a plurality of pumps each having a corresponding one of a plurality of pistons and a corresponding one of a plurality of cylinders are driven by one motor to draw and pump solvent simultaneously into corresponding columns. To form a gradient, the pumps are connected to two-way valves that are connected alternately to a first solvent and a second solvent, whereby the time said valve is in a first position controls the amount of solvent drawn from the first reservoir into said pumps and the amount of time in said second position controls the amount of said second solvent drawn from the second reservoir into said pumps and the solvent is mixed in the pumping systems. The detectors are photodiodes mounted to light guides in the flow cells that generate signals related to light absorbance and communicate with a controller, whereby the controller receives signals indicating solute between the light guides and causes collection of solute.

Abstract: A parallel fluid processing system including multiple fluid process regions containing solid material in fluid communication with a common first fluid source may be used to conduct analyses and/or synthesis in parallel. A parallel fluid processing data correction method includes supplying and processing a calibrant in each fluid process region, measuring a first physical parameter and deriving at least one correction factor based on the parameter, supplying and processing at least one second fluid in each fluid process region, and then applying the correction factor to yield corrected process data. Retention time correction, peak area correction, and other useful data corrections may be performed. Parallel fluid processing may be performed with microfluidic devices and systems. A system for correcting retention times in parallel liquid chromatography is further provided.

Abstract: A multi-layer microfluidic separation device comprises a polymeric membrane frit that may be securely bonded within the device and minimizes lateral wicking. Stationary phase material having an average particle size is retained by a frit having an average pore size that is smaller than the average particle size. In one embodiment, a secure bond is ensured by treating the polymer to match its surface energy to that of the materials to which it is bound. Treatments include plasma treatment, irradiation and the application of acids.

Abstract: The present invention exploits the discovery that amounts of uracil and thymine metabolites, especially ?-aminoisobutyric acid, in various bodily fluids, especially urine, are correlated with the occurrence of epilepsy when compared to matched control subjects. Analytical and diagnostic protocols, including a novel high performance liquid chromatography system, for use in the invention are disclosed.

Abstract: The subject invention includes constituent separation apparatuses that include a fluid pathway and a pair of spaced-apart electrodes positioned within the pathway for detecting current flow within a mobile phase present in the pathway. Coupled to the pair of spaced-apart electrodes is a mix ratio determinator for determining the mix ratio of the mobile phase from the detected current flow. Also provided are methods that include contacting a mobile phase with an apparatus for separating constituents of a mobile phase, detecting the current flow of the mobile phase when the mobile phase is in contact with the apparatus and determining the mix ratio of the mobile phase from the detected current flow. The mix ratio may be adjusted based on the determined mix ratio. Algorithms for practicing the subject methods are also provided on computer readable mediums. Systems and kits for practicing the subject methods are also provided.

Abstract: A method for analyzing a multi-channel chromatogram is realized for accurately resolving overlapping peaks on a multi-channel chromatogram to permit analysis of the composition of a sample. First, components of overlapping peaks are specified. A data matrix Dij is determined, and compressed in the wavelength direction to obtain a data matrix vector Di. Next, the two-dimensional data is deconvoluted, final standard deviation s0 is registered, and the deconvoluted two-dimensional data is reconvoluted to a retention intensity matrix. A quantitative spectral intensity matrix is computed, components are identified, and the identified components are quantified. Subsequently, an eigenvalue problem is solved, and the number n of components is estimated. The deconvolution and computation of the eigenvalue problem are iteratively executed until the peaks are isolated. Then, elution profiles are calculated, the components are identified, and the identified components are quantified.

Abstract: Numerous embodiments of a method to assay sacrificial material are disclosed. In one embodiment, a sacrificial material may be analyzed by high performance liquid chromatography. Chemical markers that correlate with material contaminants in the sacrificial material may be identified.

Abstract: A threadless interface for a fluidic system includes a microfluidic device having an outer surface and an internal near-surface channel having a first width and disposed at a first depth relative to the outer surface, with the first width being less than about two times the first depth. A fluidic seal engages the outer surface and exerts an elevated contact pressure against at least a portion of the outer surface without substantially occluding the channel. A preferred seal includes a raised boss. A fault tolerant flow path design can accommodate misalignment between adjacent device layers without detrimentally affecting fluid flow capability. The interface may be used in a microfluidic system for performing parallel analyses such as high performance liquid chromatography.

Abstract: A hyphenated technique based on the combination of high performance liquid chromatography (HPLC), electrochemical (coulometric) oxidation (EC) and electrospray ionization (ESI)- or atmospheric pressure chemical ionization (APCI)-mass spectrometry (MS), allows access of selected groups of low and medium polarity analytes to ESI- or APCI-mass spectrometry after HPLC by electrochemical treatment of the sample.

Abstract: Microfluidic analytical devices and systems have at least one porous element disposed downstream of one or more optical detection regions in a pressure-based separation system. A porous element elevates the backpressure within an optical detection region, thus suppressing bubble formation and enhancing optical detection. Various types of porous elements include porous membranes, packed particulate material, and polymerized monoliths. Preferred devices may be fabricated with substantially planar device layers, including stencil layers, that are directly bonded without adhesives to form a substantially sealed microstructure suitable for performing pressure-based chromatographic separations at elevated operating pressures and with organic solvents.

Abstract: The instrument cold sprays a solution sample at a low temperature and desolvates the sample. Under this condition, a mass analysis is performed. The instrument comprises a needle pipe (8) through which the solution sample is passed, a sheath tube (24) formed coaxially with the needle pipe (8) and passing a temperature-controlled nebulizing gas therethrough, the above-described desolvation block (3), means for cooling the block (15), means for heating the block (4), and a temperature sensor (5) for detecting the temperature of the block (3). The block (3) has a passage for charged liquid droplets of the solution sample cold sprayed from the tip of the needle pipe (8), and acts to remove the solvent from the charged liquid droplets flowing through the passage. A coldspray mass spectrometer is offered which has a desolvation block whose temperature can be easily controlled. In the instrument, condensation of water and electrical leakage are prevented for a long time.

Abstract: High throughput liquid chromatography systems include multiple separation columns and multiple flow-through detection regions in sensory communication with a common radiation source and a multi-channel detector. Preferred detector types include a multi-anode photomultiplier tube, a charge-coupled device detector, a diode array, and a photodiode array. In certain embodiments, separation columns are microfluidic and integrated into a unitary microfluidic device. The optical path through a detection region is preferably coaxial with the path of eluate flow along a flow axis through a detection region. On-board or off-board detection regions may be provided.

Abstract: Pressure-driven microfluidic separation devices, such as may be used for performing high performance liquid chromatography, are provided. Multiple separation columns may be defined in a single device and packed with stationary phase material retained by porous frits. One or more splitters may be provided to distribute slurry and/or mobile phase among multiple separation columns. In one embodiment, separation devices are substantially planar and fabricated with multiple device layers. Systems and methods employing slurry for packing separation devices are also provided.

Abstract: The invention relates to a temperature-controlled injector for a chemical analysis unit, in particular a gas chromatograph, comprising an injector tube, which can be received by a receiving tube, having a cooling system, which surrounds the receiving tube, through which coolant can flow, which has coolant connections and which is designed as a metallic tube coil, and a resistance heating system for the injector tube, in which injector the receiving tube consists of a material of good thermal conductivity, is electrically insulating towards the outside, and the tube coil rests on the receiving tube, has an electrical resistance which is sufficient to rapidly heat the injector tube and can be acted on by current via electrical connection pieces.

Abstract: To economically perform preparatory chromatography, a plurality of pumps each having a corresponding one of a plurality of pistons and a corresponding one of a plurality of cylinders are driven by one motor to draw and pump solvent simultaneously into corresponding columns. To form a gradient, the pumps are connected to two-way valves that are connected alternately to a first solvent and a second solvent, whereby the time said valve is in a first position controls the amount of solvent drawn from the first reservoir into said pumps and the amount of time in said second position controls the amount of said second solvent drawn from the second reservoir into said pumps and the solvent is mixed in the pumping systems. The detectors are photodiodes mounted to light guides in the flow cells that generate signals related to light absorbance and communicate with a controller, whereby the controller receives signals indicating solute between the light guides and causes collection of solute.

Abstract: Methods for capturing analytes associated with surface-bound ligands are disclosed. The methods involve eluting analytes from surface-bound ligands with a first liquid to generate free analytes, and capturing the free analytes with a solid capturing material within the first liquid to generate a first liquid containing captured analytes. The first liquid may be a flowing liquid or a non-flowing liquid, and the surface to which the surface-bound ligand is attached may be a sensing surface, such as a biosensor, or a non-sensing surface. The captured analytes may be further consolidated at a location removed from the surface-bound ligand, eluted from the solid capturing material with a second liquid, and used for subsequent analysis or procedures.

Abstract: To provide a method of and an apparatus for continuously measuring elemental mercury and bivalent mercury both contained in a gaseous medium fractionally with a simplified structure, the concentration of a total mercury (Metallic Mercury+Bivalent Mercury) and the concentration of elemental mercury contained in gases are measured continuously and fractionally. In the practice of this mercury measuring method, a first column 1, filled with a first fixed catalyst, and a second column 11, filled with a second fixed catalyst, are fluid connected in parallel relation to each other. The gases G are introduced into those first and second columns 1 and 11. In the first column 1, the first fixed catalyst collects and removes the bivalent mercury, but passes only the elemental mercury in the gases through the first column.

Abstract: A frit for use in multi-layer microfluidic separation devices is provided. The frit comprises a polymeric membrane that may be securely bonded within the device and minimizes lateral wicking. A secure bond is ensured by treating the polymer to match its surface energy to that of the materials to which it is bound. Treatments include plasma treatment, irradiation and the application of acids.

Abstract: A closure cap system for glass chromatography columns includes a glass cylinder with unfinished shaping or work on each end, and two sealing caps. The caps have a circumference shoulder with O-rings. The O-rings having the same diameter as the diameter of the glass cylinder unfinished ends. A base and top parts, both containing openings for receiving sealing caps and the glass cylinder. Threaded rods are received by additional openings in said top and base parts. Nuts are affixed at the end of each threaded rod. The combined action of the nuts and threaded rods apply compression forces to the caps and glass cylinder for sealing in a simple and economic manner defining the system as a disposable apparatus.

Abstract: Microfluidic analytical devices and systems have at least one porous element disposed downstream of one or more optical detection regions in a pressure-based separation system. A porous element elevates the backpressure within an optical detection region, thus suppressing bubble formation and enhancing optical detection. Various types of porous elements include porous membranes, packed particulate material, and polymerized monoliths. Preferred devices may be fabricated with substantially planar device layers, including stencil layers, that are directly bonded without adhesives to form a substantially sealed microstructure suitable for performing pressure-based chromatographic separations at elevated operating pressures and with organic solvents.

Abstract: A system for separating an aqueous stream of mixed polynucleotides into a series of length-based polynucleotide fractions and collecting one or more of the length-based polynucleotide fractions into separate containers. The system comprises a separation column containing separation media for separating an aqueous stream of mixed polynucleotides into a series of length-based polynucleotide fractions; a container including one or more single-sample containers; an ejection chamber having a separated sample inlet for receiving the length-based polynucleotide fractions, a waste outlet for discharging uncollected sample, and a capillary-sized fraction outlet positioned to discharge a selected length-based polynucleotide fraction into a single-sample container. The system also includes means for effecting discharge of a selected length-based polynucleotide fraction into the separate container.

Abstract: Methods and apparatus for the evaluation of interactions between substances using inverse chromatography are disclosed. Preferably, interactions are evaluated between a liquid test sample and a solid phase comprising a receptor in the presence of a liquid carrier. Preferably, one of the modifying agent or receptor are members of a combinatorial library.

Abstract: The present invention comprises a device and method of analyzing trace amounts of perchlorate in liquid samples comprising a concentrator column used in an ion chromatographic system that comprises an anionic capacity ranging from about 0.030 microequivalents per column to about 0.060 microequivalents per column and capable of removing substantially all perchlorate from the sample and using a multi-directional flow through said concentrator column in order to enhance perchlorate detection. The invention also comprises a packing material comprising from about 25 percent to about 80 percent of a low anionic capacity material comprising an anionic capacity of less than about 0.03 milliequivalents per milliliter mixed with from about 25 percent to about 80 percent of a high anionic capacity material comprising a anionic capacity of more than about 0.07 milliequivalents per milliliter.

Abstract: Apparatus for separating the components of a sample by OPLC type chromatography using liquid under pressure, the apparatus comprises a stationary phase forming one or more sample treatment paths and means for feeding moving phase to one end of the stationary phase, with means at the opposite end of the stationary phase for collecting moving phase, means for injecting moving phase also being provided at the sides of the stationary phase in order to eliminate edge effects in the fronts of sample components and in order to separate treatment paths from one another.

Abstract: The invention relates to a chromatography device comprising: