WO2013008502A1 - 固相抽出装置および粘度測定装置 - Google Patents
固相抽出装置および粘度測定装置 Download PDFInfo
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- WO2013008502A1 WO2013008502A1 PCT/JP2012/060204 JP2012060204W WO2013008502A1 WO 2013008502 A1 WO2013008502 A1 WO 2013008502A1 JP 2012060204 W JP2012060204 W JP 2012060204W WO 2013008502 A1 WO2013008502 A1 WO 2013008502A1
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- phase extraction
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
- B01L3/02—Burettes; Pipettes
- B01L3/021—Pipettes, i.e. with only one conduit for withdrawing and redistributing liquids
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/405—Concentrating samples by adsorption or absorption
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/02—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor using a plurality of sample containers moved by a conveyor system past one or more treatment or analysis stations
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L2200/00—Solutions for specific problems relating to chemical or physical laboratory apparatus
- B01L2200/14—Process control and prevention of errors
- B01L2200/143—Quality control, feedback systems
- B01L2200/146—Employing pressure sensors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L2200/00—Solutions for specific problems relating to chemical or physical laboratory apparatus
- B01L2200/14—Process control and prevention of errors
- B01L2200/148—Specific details about calibrations
Definitions
- the present invention relates to a solid-phase extraction apparatus for purifying or concentrating a measurement component in a sample solution using a solid-phase extraction cartridge having a solid-phase extraction material therein, and in particular, by introducing pressurized air into the solid-phase extraction cartridge.
- the present invention relates to pressure control based on the viscosity of a sample solution in pressure extraction for solid phase extraction.
- Solid phase extraction is a method of separating measurement components and impurities in a sample solution based on physical and chemical properties using a solid (solid phase extraction material) generally called a stationary phase. Solid phase extraction is used for the purpose of purifying a measurement component by removing impurities that interfere with analysis in various analysis techniques (liquid chromatography, mass spectrometry).
- Samples used for analysis include urine, blood, water, and soil.
- the sample solution passes through the solid-phase extraction material, if the affinity between the measurement component and the solid-phase extraction material surface is high, the measurement component of the sample solution is selectively adsorbed, so the measurement component is purified or concentrated. be able to.
- organic polymer particles such as silica gel and styrene-divinylbenzene copolymer, or those obtained by chemically modifying the surface of these particles.
- the solid-phase extraction process consists of an adsorption process that adsorbs the measurement components in the sample solution to the solid-phase extraction material, a washing process that cleans impurities other than the measurement components adsorbed on the solid-phase extraction material, and an adsorption to the solid-phase extraction material. It consists of three elution steps for eluting the measurement components.
- Measured components are adsorbed in the adsorption process, and components (impurities) that interfere with analysis flow out without being adsorbed. This is the first purification step. However, since there are impurities that are adsorbed on the solid phase extraction material, the adsorbed impurities are removed in the cleaning step. This is the second purification step.
- the purified measurement component is separated from the solid phase extraction material by the eluate. Further, the separated extract is sent to the analyzer and the signal intensity of the measurement component is measured. As described above, in solid phase extraction, impurities are removed in the order of adsorption, washing, and elution steps, and the measurement component is purified.
- a solid-phase extraction material is disclosed in which pressure is applied to a sample solution using a pressurizing mechanism described in JP-A-8-164302 (Patent Document 1). And a solid-phase extraction apparatus in which a sample solution passes through a solid-phase extraction material using a decompression mechanism described in JP-A-2006-7081 (Patent Document 2).
- Patent Document 3 an extraction apparatus described in Japanese Patent Application Laid-Open No. 2005-110670 (Patent Document 3) that determines a pressurization condition in accordance with information corresponding to the type of sample liquid in advance. There was also.
- the rate at which the measurement component of the sample solution is adsorbed on the solid phase extraction material greatly depends on the speed at which the sample solution passes through the solid phase extraction material.
- the viscosity of the sample solution used for solid-phase extraction is not constant, so the flow rate in the adsorption process fluctuates, the adsorption rate varies, and the accuracy of the recovery of the measured components in the elution process also decreases. End up.
- the recovery rate is a ratio of the amount of the measurement component after the elution step and the amount of the measurement component in the sample solution.
- the sample liquid is pressurized and extracted at a pressure set in advance by the operator.
- a pressure set in advance In order to obtain a stable recovery rate and processing capacity of the measurement components with this solid-phase extraction device, it is necessary to measure the viscosity of the sample solution in advance using another measuring device such as a viscometer. , And increase in labor costs.
- the decompression method is used in the solid phase extraction of the apparatus described in Patent Document 2.
- a sample solution, a reagent, and the like are dispensed into a multi-well cartridge equipped with a solid phase extraction material, and suction extraction is performed.
- suction extraction is performed.
- the sample liquids of a plurality of wells are simultaneously aspirated and extracted, the flow rate of each well varies.
- the extraction method described in Patent Document 3 is a method of changing the applied pressure according to the type and characteristics of the sample liquid. Specifically, the extraction time is shortened by increasing the pressure applied in the next washing process and elution process for the sample liquid that took a long time to transport the liquid in the adsorption process.
- This method shortens the extraction time, but does not perform an extraction process that optimizes the recovery rate of the measured components in the entire extraction process.
- the viscosity is different, and the time fluctuation is the largest among the adsorption, washing, and elution processes. Since the solution used in the washing and elution processes is a reagent and the viscosity is substantially constant, increasing the applied pressure leads to a decrease in the recovery rate of the measurement component.
- Patent Document 3 since the pressure of the washing and elution processes is controlled using the liquid feeding time of the adsorption process, the flow rate is controlled so that the recovery rate of the measurement component in the adsorption process is optimized. It is impossible. For this reason, even in this apparatus, when the viscosity of the sample solution is different, the ratio of adsorption of the measurement component varies, and the accuracy of the recovery rate of the measurement component is lowered.
- the object of the present invention is to improve the accuracy of the recovery rate of the measured components even in the measurement for each sample solution having different viscosities, and to ensure a certain processing capacity.
- the outline of a representative one is that in a solid-phase extraction apparatus, pressure is applied to a sample dispensing unit that dispenses a sample solution and a sample solution dispensed by the sample dispensing unit, and a measurement component is extracted from the sample solution.
- a solid-phase extraction unit that performs a solid-phase extraction process for extraction and a conversion unit that measures the viscosity of the sample liquid and determines the pressure based on the measured viscosity information of the sample liquid are provided.
- a pressurizing syringe pump In the solid phase extraction apparatus, a pressurizing syringe pump, an air supply tube, an air supply tube pressure sensor, a solenoid valve, a solid phase extraction cartridge, a sample dispensing nozzle, a sample dispensing syringe pump, A liquid pipe, a pressure sensor for the liquid feeding pipe, and a control unit, the control unit calculates the viscosity of the sample liquid based on the pressure measured by the pressure sensor for the liquid feeding pipe, and information on the calculated viscosity of the sample liquid Based on the above, the pressure to be applied to the solid phase extraction cartridge is determined and controlled with high accuracy without reducing the recovery rate of the measurement component from the sample liquid.
- a sample dispensing nozzle that sucks and discharges the sample liquid
- a sample dispensing syringe pump that performs the suction and discharge operations of the sample liquid
- a sample dispensing nozzle and a sample dispensing syringe pump
- a liquid feeding pipe to be connected a pressure sensor for a liquid feeding pipe that measures the pressure in the liquid feeding pipe, and a conversion unit that calculates viscosity information of the sample liquid based on the pressure measured by the pressure sensor for the liquid feeding pipe It is.
- the effect obtained by a typical one is that the viscosity of the sample liquid can be accurately measured by monitoring the pressure in the liquid feeding tube during the suction of the sample liquid, and depending on the measured viscosity, By adjusting the pressure applied to each step of washing and elution, an accurate flow rate can be controlled. As a result, the flow rate can be kept constant without being affected by the viscosity of the sample solution, and a certain treatment capacity can be secured. Furthermore, a stable recovery rate of the measurement component is obtained, and the analysis accuracy is improved.
- FIG. 1 It is a block diagram which shows schematic structure of the solid-phase extraction apparatus which concerns on one embodiment of this invention. It is a block diagram which shows the whole structure of the solid-phase extraction apparatus which concerns on one embodiment of this invention. It is explanatory drawing for demonstrating operation
- (A)-(c) is a figure which shows the relationship between the liquid flow rate in the pressurization control at the time of the solid-phase extraction process of the solid-phase extraction apparatus which concerns on one embodiment of this invention, and the recovery rate of a measurement component.
- (A), (b) is explanatory drawing for demonstrating the measuring method of the viscosity by the viscosity measurement part of the solid-phase extraction apparatus which concerns on one embodiment of this invention. It is explanatory drawing for demonstrating the specific structure of the viscosity measurement part and pressurized air supply part of the solid-phase extraction apparatus which concerns on one embodiment of this invention. It is a flowchart which shows the pressurization control process of the solid-phase extraction apparatus which concerns on one embodiment of this invention.
- FIG. 1 is a block diagram showing a schematic configuration of a solid phase extraction apparatus according to an embodiment of the present invention.
- a solid phase extraction apparatus 100 is composed of a viscosity measurement unit 3, a conversion unit 4, a sample dispensing unit 5, and a solid phase extraction unit 6, and a sample container 2 containing a sample solution 1 is installed to form a solid phase. Perform extraction.
- the sample container 2 containing the sample liquid 1 is installed in the solid phase extraction apparatus 100, and the viscosity of the sample liquid 1 is measured by the viscosity measuring unit 3.
- the conversion unit 4 calculates the pressure used for the solid phase extraction based on the information measured by the viscosity measurement unit 3.
- the sample solution 1 is fed to the solid phase extraction unit 6 through the sample dispensing unit 5.
- the solid phase extraction is performed by applying the pressure calculated by the conversion unit 4 and reducing the pressure.
- FIG. 2 is a block diagram showing the overall configuration of the solid-phase extraction apparatus according to one embodiment of the present invention, and shows a plan view.
- a solid phase extraction apparatus 100 includes a panel display unit 101 with an operation panel, an input unit 102, a calculation processing unit 103, a storage unit 104, an external communication interface unit 105 that performs communication processing with the outside, and a sample that undergoes extraction processing.
- Sample container 2 into which the liquid is dispensed sample installation unit 106 in which the sample container 2 is arranged, solid phase extraction cartridge 107, extraction container 108, installation for storing the solid phase extraction cartridge 107 and the extraction container 108 before use 109, a processing unit 110 that performs a solid phase extraction process using the solid phase extraction cartridge 107, a reagent container 111 that stores a cleaning solution and an eluate used for the solid phase extraction process, a reagent placement unit 112 that arranges the reagent container 111, Sample dispensing mechanism 113 (sample dispensing unit 5) for dispensing a sample to a solid-phase extraction cartridge, and reagent dispensing for dispensing a reagent to a solid-phase extraction cartridge Mechanism 114, solid phase extraction processing unit 115 (solid phase extraction unit 6) for performing extraction processing, extraction container setting unit 116 in which an extraction container is disposed, extraction sample liquid dispensing mechanism 117 and mechanism for dispensing extracted sample liquid It is comprised from the control unit 118
- a detection unit 119 for measuring a measurement component using an extraction sample subjected to solid phase extraction is connected.
- the detector 119 may be a detector applicable for measuring an object, and may be a photometer, a mass spectrometer, or other detectors.
- FIG. 3 is an explanatory diagram for explaining the operation of the solid phase extraction of the solid phase extraction apparatus according to the embodiment of the present invention.
- a solid-phase extraction material 202 is sealed inside a solid-phase extraction cartridge 107 used in the solid-phase extraction apparatus 100.
- the solid phase extraction apparatus 100 sequentially moves the cartridge by moving the processing unit 110 in which the solid phase extraction cartridge 107 is installed, and the sample liquid input by the operator through the input unit 102 of the solid phase extraction apparatus 100 or the panel display unit 101. Based on information such as 1, a dispensing amount of sample liquid 1 in accordance with the extraction conditions stored in the apparatus is sucked from the sample container 2 by the sample dispensing nozzle 201 of the sample dispensing mechanism 113, and a solid phase extraction cartridge Dispense to 107.
- the solid phase extraction cartridge 107 that has received the dispensing of the sample solution 1 moves to the solid phase extraction processing unit 115.
- the processing unit 110 since the processing unit 110 has a circular table shape, the movement is performed by a rotational motion.
- the solid phase extraction processing unit 115 air is supplied after the solid phase extraction cartridge 107 and the extraction nozzle 203 are joined.
- the sample liquid 1 passes through the solid phase extraction material 202, and the measurement component is adsorbed by the solid phase extraction material 202. At this time, the impurities are drained. Next, the solid phase extraction cartridge 107 undergoes a cleaning process in a state where the measurement component is adsorbed on the solid phase extraction material 202.
- the cleaning reagent in the reagent container 111 is sucked by the reagent dispensing mechanism 114 and discharged to the solid phase extraction cartridge 107.
- the discharged cleaning reagent passes through the solid-phase extraction material 202 by supplying air from the extraction nozzle 203 of the solid-phase extraction processing unit 115.
- the eluate is aspirated from the reagent container 111 by the reagent dispensing mechanism 114 and discharged to the solid phase extraction cartridge 107.
- the discharged eluate passes through the solid-phase extraction material 202 and elutes the measurement component by supplying air from the extraction nozzle 203 of the solid-phase extraction processing unit 115.
- the extraction sample liquid is received by the lower extraction container 108.
- the extraction container 108 moves the extraction container to the position of the extraction sample liquid dispensing mechanism 117 by the movement of the extraction container installation unit 116, where the extraction sample liquid in the extraction container 108 is sent to the detection unit 119, Detect the measurement component.
- the output of the detection unit 119 is displayed on the panel display unit 101 as a desired measurement result after being subjected to concentration calculation, unit conversion processing, and the like by the calculation processing unit 103, and is stored in the storage unit 104 together with sample information.
- An extracted sample solution containing the measurement component can be obtained by such a series of solid-phase extraction operations.
- the content of a measurement component is measured by measuring an extracted sample solution from which impurities in the sample are removed by a solid-phase extraction using a measuring instrument such as a photometer or a mass spectrometer.
- Pressurization by supplying air from the extraction nozzle 203 in the above processing is controlled by the conversion unit 4 and the control unit 118 based on the viscosity of the sample by the viscosity measuring unit 3 shown in FIG.
- pressurization control will be described.
- FIG. 4 is a diagram showing the relationship between the flow rate and the recovery rate of the measurement component in the pressurization control during the solid phase extraction process of the solid phase extraction apparatus 100 according to one embodiment of the present invention. ) Shows the adsorption process, FIG. 4 (b) shows the washing process, and FIG. 4 (c) shows the elution process. The horizontal axis is the flow rate proportional to the pressure of pressurization, and the vertical axis is the recovery rate of the measured component. is there.
- the measured component cannot be adsorbed if the liquid flow rate is too high. Therefore, the recovery rate monotonously decreases as the liquid passing speed increases.
- the recovery rate of all processes is the multiplication of FIG. 4 (a), FIG. 4 (b), and FIG. 4 (c), and has a liquid passing speed that provides an optimal recovery rate for each measurement component.
- the flow rate in each step and the recovery rate of the measured component depends on the affinity between each measured component and the solid-phase extractant and solvent, the flow rate must be controlled for each measured component. It becomes.
- the flow rate of the three steps is independently controlled and optimized.
- the flow rate is inversely proportional to the viscosity and proportional to the pressure, as is known from the Poiseuille equation.
- the viscosity of the sample solution 1 is measured, and the pressure applied to the sample solution 1 by solid phase extraction is determined based on the measured value. Part 4) is calculated and controlled. Specifically, as shown in FIG. 4A, when the viscosity is high, the pressure to be applied is increased, and when the viscosity is low, the pressure to be applied is decreased to approach the target liquid passing speed.
- the recovery rate of the measured component can be optimized.
- FIG. 4 shows an example in which the recovery rate of the measurement component decreases as the flow rate increases in the adsorption step and the elution step, and the recovery rate of the measurement component increases as the flow rate increases in the washing step.
- the flow rate of the three steps is controlled independently. By optimizing, it is possible to optimize the recovery rate.
- FIG. 5 is an explanatory diagram for explaining a viscosity measurement method by the viscosity measurement unit of the solid-phase extraction apparatus 100 according to an embodiment of the present invention.
- the axis is the output of the pressure sensor indicating the pressure in the sample dispensing nozzle 201.
- the horizontal axis represents the viscosity
- the vertical axis represents the maximum value of the negative pressure detected with the passage of the measurement time in FIG.
- the viscosity of the sample liquid 1 is calculated from the pressure in the sample dispensing nozzle 201.
- the pressure in the sample dispensing nozzle 201 becomes a negative pressure, and the maximum value of the negative pressure according to the viscosity. And the time to return to the steady state is different.
- the maximum value of the measured negative pressure the difference between the atmospheric pressure and the maximum value of the measured negative pressure, the time until the steady state is reached, or the pressure until the steady state is reached.
- the viscosity of the sample liquid 1 is calculated from the integrated value of the waveform.
- the maximum value of the negative pressure in the sample dispensing nozzle 201 has a relationship as shown in FIG. 5B, for example, and the viscosity is a control unit according to the maximum value of the negative pressure in the sample dispensing nozzle 201. It is calculated from the function stored in 118.
- the conversion unit 4 in the control unit 118 determines the pressure to be applied according to the viscosity calculated by the conversion unit 4 in the control unit 118 so as to optimize the recovery rate of the measurement component, and controls the flow rate. To do.
- the example of the maximum value of the negative pressure is shown.
- the difference between the atmospheric pressure and the measured maximum value of the negative pressure, the time until the steady state is reached, the steady state The integrated value of the pressure waveform up to becomes also related to the viscosity, and the viscosity can be calculated by storing these in the control unit 118 or the conversion unit 4 as a function.
- a viscometer or other measuring device may be used as a measuring device for measuring the viscosity of the sample solution 1.
- FIG. 6 is an explanatory diagram for explaining specific configurations of the viscosity measurement unit and the pressurized air supply unit of the solid-phase extraction apparatus 100 according to the embodiment of the present invention, and is a control system of the pressurized air supply mechanism. The figure is shown.
- the pressurized air supply mechanism 200 connects a sample dispensing nozzle 201, a sample dispensing syringe pump 301 for sucking the sample liquid 1, a sample dispensing syringe pump 301, and the sample dispensing nozzle 201.
- Liquid feed pipe 302 liquid feed pipe pressure sensor 303 for measuring the pressure in the sample dispensing nozzle 201, pressurizing syringe pump 306 for applying pressure, and extraction nozzle for feeding air to the solid phase extraction cartridge 107 203, an air supply pipe 308 that connects the pressurizing syringe pump 306 and the extraction nozzle 203, an air supply pipe pressure sensor 307 that measures the pressure in the air supply pipe 308, and an electromagnetic valve 305 that maintains the pressure in the air supply pipe 308 at a high pressure.
- An electrical signal is represented by 304.
- sample dispensing nozzle 201 the sample dispensing syringe pump 301, the liquid feeding pipe 302, the liquid feeding pipe pressure sensor 303, the control unit 118, the conversion unit 4, and the panel display unit 101 with an operation panel constitute a viscosity measuring apparatus. ing.
- the viscosity measuring unit 3 in FIG. 1 corresponds to a pressure measurement by the liquid pipe pressure sensor 303 and a viscosity calculation process by the conversion unit 4 in the control unit 118 based on the measured value.
- the conversion part 4 was installed in the control unit 118, the conversion part 4 may exist in the pressure sensor 303 for liquid feeding pipes, or another place. Furthermore, it is assumed that a plurality of conversion units 4 may exist.
- FIG. 7 is a flowchart showing the pressurization control process of the solid phase extraction apparatus 100 according to the embodiment of the present invention.
- pressurization control is started (S30).
- An electric signal 304 of an input value from the panel display unit 101 or the input unit 102 is converted into a driving amount of the sample dispensing syringe pump 301 by the control unit 118 and sent to the sample dispensing syringe pump 301 as an electric signal 304. .
- the sample dispensing syringe pump 301 is driven according to the drive amount of the electric signal 304, and sucks the sample liquid 1 from the sample dispensing nozzle 201 (S31).
- the pressure P 1 in the liquid feeding pipe 302 is measured by the pressure sensor 303 for the liquid feeding pipe, and the electric signal 304 of the pressure P 1 is transmitted to the conversion unit 4 in the control unit 118 (S32). .
- the sample dispensing nozzle 201 discharges the sucked sample liquid 1 into the solid phase extraction cartridge 107.
- the conversion unit 4 in the control unit 118 calculates the viscosity ⁇ based on the value of the pressure P 1 received from the liquid feed pipe pressure sensor 303 and applies it to the sample liquid 1 dispensed in the solid phase extraction cartridge 107. determining the drive amount of the pressure P 2 and pressurizing the syringe pump 306 (S33).
- the pressure P 2 is the product of the liquid flow velocity v and the viscosity ⁇ of the sample liquid 1 at which the recovery rate for each measurement component stored in the conversion unit 4 in the control unit 118 is optimized.
- control unit 118 transmits an electric signal 304 to the electromagnetic valve 305, and closes the electromagnetic valve 305 (S34).
- the electric signal 304 of the driving amount of the pressurizing syringe pump 306 is transmitted to the pressurizing syringe pump 306, the pressurizing syringe pump 306 is driven, and the pressure in the air supply pipe 308 is increased (S35).
- the pressure P 3 in the air supply pipe 308 is measured by the air supply pipe pressure sensor 307, and the electric signal 304 of the pressure P 3 is transmitted to the control unit 118 (S36).
- the control unit 118 determines whether the difference between the pressure P 2 is applied to the pressure P 3 is in within ⁇ 5% of P 2 (P 2 -P 2 ⁇ 5% ⁇ P 3 ⁇ P 2 + P 2 ⁇ 5 %) (S37).
- the driving amount of the pressurizing syringe pump 306 is determined again, and the driving amount electric signal 304 is transmitted from the control unit 118 to the pressurizing syringe pump 306, thereby increasing the pressure in the air supply pipe 308. Alternatively, it is lowered (S35).
- the viscosity ⁇ of the sample liquid 1 is calculated, and the pressure to be applied is determined based on the calculated viscosity ⁇ information and the information on the flow rate at which the recovery rate of the measured component is optimal. By doing so, it is possible to optimize the recovery rate of the measurement component.
- the applied pressure is the recovery rate of the plurality of measurement components.
- the pressure can be controlled so that the difference between the two becomes the smallest, or the applied pressure can be controlled so that the average of the recovery rates of the plurality of measurement components becomes the largest.
- the present invention relates to a solid-phase extraction apparatus for purifying or concentrating a measurement component in a sample solution using a solid-phase extraction cartridge having a solid-phase extraction material inside, and relates to solid phase extraction by introducing pressurized air into the solid-phase extraction cartridge.
- the present invention can be widely applied to apparatuses and systems that perform pressure control in pressure extraction for phase extraction.
- Solid phase extraction processing unit 116 ... Extraction container installation unit, 117 ... Extracted sample liquid dispensing mechanism , 118 ... control unit, 119 ... detection unit, 200 ... pressurized air supply mechanism, 201 ... sample dispensing nozzle, 202 ... solid phase extraction material, 203 ... extraction nozzle, 301 ... syringe pump for sample dispensing, 302 ... sending liquid , 303 ... pressure sensor liquid feed pipe, 304 ... electric signal, 305 ... electromagnetic valve, 306 ... pressurizing syringe pump, 307 ... flue pressure sensor, 308 ... flue.
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Abstract
Description
図1により、本発明の一実施の形態に係る固相抽出装置の概略構成について説明する。図1は本発明の一実施の形態に係る固相抽出装置の概略構成を示すブロック図である。
次に、図2により、本発明の一実施の形態に係る固相抽出装置の全体構成について説明する。図2は本発明の一実施の形態に係る固相抽出装置の全体構成を示す構成図であり、平面図を示している。
次に、図2および図3により、本発明の一実施の形態に係る固相抽出装置の固相抽出の動作について説明する。図3は本発明の一実施の形態に係る固相抽出装置の固相抽出の動作を説明するための説明図である。
次に、図4により、本発明の一実施の形態に係る固相抽出装置100の固相抽出処理時の加圧制御における通液速度と測定成分の回収率との関係について説明する。図4は本発明の一実施の形態に係る固相抽出装置100の固相抽出処理時の加圧制御における通液速度と測定成分の回収率との関係を示す図であり、図4(a)は吸着工程、図4(b)は洗浄工程、図4(c)は溶出工程を示し、横軸が加圧の圧力に比例している通液速度、縦軸が測定成分の回収率である。
次に、図5により、本発明の一実施の形態に係る固相抽出装置100の粘度測定部による粘度の測定方法について説明する。図5は本発明の一実施の形態に係る固相抽出装置100の粘度測定部による粘度の測定方法を説明するための説明図であり、図5(a)は、横軸が測定時間、縦軸が試料分注ノズル201内の圧力を示す圧力センサの出力である。図5(b)は、横軸が粘度、縦軸が図5(a)の測定時間の経過により検出した負圧の最大値である。
次に、図6により、本発明の一実施の形態に係る固相抽出装置100の粘度測定部および加圧エア供給部の具体的な構成について説明する。図6は本発明の一実施の形態に係る固相抽出装置100の粘度測定部および加圧エア供給部の具体的な構成を説明するための説明図であり、加圧エア供給機構の制御系統図を示している。
次に、図6および図7により、本発明の一実施の形態に係る固相抽出装置100の加圧制御処理について説明する。図7は本発明の一実施の形態に係る固相抽出装置100の加圧制御処理を示すフローチャートである。
Claims (6)
- 試料液を分注する試料分注部と、
前記試料分注部で分注された前記試料液に圧力を印加し、前記試料液から測定成分を抽出する固相抽出処理を行う固相抽出部と、
前記試料液の粘度を測定し、測定された前記試料液の粘度の情報に基づいて、前記圧力を決定する換算部とを備えたことを特徴とする固相抽出装置。 - 請求項1に記載の固相抽出装置において、
前記換算部は、前記試料分注部での前記試料液の吸引時の負圧の最大値、大気圧と前記負圧の最大値との差、前記試料液の吸引後に定常状態になるまでの時間、または前記定常状態になるまでの圧力波形の積分値の情報に基づいて、前記粘度を測定することを特徴とする固相抽出装置。 - 空気の吸引および吐出動作を行う加圧用シリンジポンプと、
前記空気を送気する送気管と、
前記送気管内の圧力をモニタリングする送気管用圧力センサと、
前記送気管内の圧力を高圧に保持するための電磁弁と、
固相抽出材を備えた固相抽出カートリッジと、
試料液の吸引および吐出を行う試料分注ノズルと、
前記試料液の吸引および吐出動作を行う試料分注用シリンジポンプと、
前記試料分注ノズルと前記試料分注用シリンジポンプを繋ぐ送液管と、
前記送液管内の圧力を測定する送液管用圧力センサと、
前記試料分注用シリンジポンプを動作させ、前記試料分注ノズルから前記試料液を吸引させて、前記試料液を前記固相抽出カートリッジに吐出し、前記加圧用シリンジポンプを動作させ、前記空気を前記固相抽出カートリッジに送気して圧力を印加し、前記試料液から測定成分を抽出する固相抽出処理を行う制御ユニットとを備え、
前記制御ユニットは、前記送液管用圧力センサで測定された圧力に基づいて前記試料液の粘度情報を得て、前記試料液の粘度の情報に基づいて、前記固相抽出カートリッジへ印加する圧力を決定する換算部を有することを特徴とする固相抽出装置。 - 請求項3に記載の固相抽出装置において、
前記換算部は、前記試料分注ノズルでの前記試料液の吸引時の負圧の最大値、大気圧と前記負圧の最大値との差、前記試料液の吸引後に定常状態になるまでの時間、または前記定常状態になるまでの圧力波形の積分値の情報に基づいて、前記粘度情報を算出することを特徴とする固相抽出装置。 - 請求項3に記載の固相抽出装置において、
前記換算部は、複数の前記測定成分を同時に抽出する際、複数の前記測定成分の回収率の差が小さくなる圧力に決定、または複数の前記測定成分の回収率の平均値が大きくなる圧力に決定することを特徴とする固相抽出装置。 - 試料液の吸引および吐出を行う試料分注ノズルと、
前記試料液の吸引および吐出動作を行う試料分注用シリンジポンプと、
前記試料分注ノズルと前記試料分注用シリンジポンプを繋ぐ送液管と、
前記送液管内の圧力を測定する送液管用圧力センサと、
前記送液管用圧力センサで測定された圧力に基づいて、前記試料液の粘度情報を算出する換算部とを備えたことを特徴とする粘度測定装置。
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CN113391000A (zh) * | 2021-07-05 | 2021-09-14 | 苏州中科国源检测技术服务有限公司 | 一种液体溶剂取样和组分分析系统 |
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