CN116879471A - Pretreatment method for enrichment of liquid phase detection sample - Google Patents
Pretreatment method for enrichment of liquid phase detection sample Download PDFInfo
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- 238000001514 detection method Methods 0.000 title claims abstract description 168
- 239000007791 liquid phase Substances 0.000 title claims abstract description 100
- 238000002203 pretreatment Methods 0.000 title claims abstract description 32
- 238000012360 testing method Methods 0.000 claims abstract description 100
- 238000000605 extraction Methods 0.000 claims abstract description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 135
- 238000010438 heat treatment Methods 0.000 claims description 75
- 239000000126 substance Substances 0.000 claims description 57
- 238000002414 normal-phase solid-phase extraction Methods 0.000 claims description 44
- 230000012447 hatching Effects 0.000 claims description 39
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 36
- 239000007788 liquid Substances 0.000 claims description 30
- 239000003153 chemical reaction reagent Substances 0.000 claims description 27
- 230000001360 synchronised effect Effects 0.000 claims description 18
- 238000002137 ultrasound extraction Methods 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 17
- 238000003260 vortexing Methods 0.000 claims description 15
- 230000010355 oscillation Effects 0.000 claims description 13
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 3
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims description 3
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 3
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 3
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 3
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 3
- 238000011534 incubation Methods 0.000 claims 2
- -1 ethylenediamine tetraacetic acid Sodium azide Chemical compound 0.000 claims 1
- 239000002904 solvent Substances 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 239000003814 drug Substances 0.000 abstract description 11
- 229940079593 drug Drugs 0.000 abstract description 11
- 238000011835 investigation Methods 0.000 abstract description 8
- 239000000523 sample Substances 0.000 description 212
- 238000002604 ultrasonography Methods 0.000 description 9
- PXIPVTKHYLBLMZ-UHFFFAOYSA-N Sodium azide Chemical compound [Na+].[N-]=[N+]=[N-] PXIPVTKHYLBLMZ-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229910001385 heavy metal Inorganic materials 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 238000004904 shortening Methods 0.000 description 3
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000012472 biological sample Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000004005 microsphere Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000008363 phosphate buffer Substances 0.000 description 2
- 239000003755 preservative agent Substances 0.000 description 2
- 230000002335 preservative effect Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 238000000622 liquid--liquid extraction Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/08—Preparation using an enricher
-
- 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
-
- 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
- G01N1/4077—Concentrating samples by other techniques involving separation of suspended solids
-
- 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
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- 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
- G01N1/4077—Concentrating samples by other techniques involving separation of suspended solids
- G01N2001/4094—Concentrating samples by other techniques involving separation of suspended solids using ultrasound
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
Abstract
The application relates to the technical field of detection, in particular to a pretreatment method for enriching a liquid phase detection sample. The pretreatment method for enrichment of the liquid phase detection sample has the advantages of simple operation, short extraction time, low cost and the like, and can be completed without specific environments and instruments such as a laboratory and the like. In addition, in some field detection, especially in drug case investigation, can shorten the detection duration greatly, and then have the advantage that testing result timeliness is good.
Description
Technical Field
The application relates to the technical field of detection, in particular to a pretreatment method for enrichment of a liquid phase detection sample.
Background
In detection analysis of some liquid phase samples, for example, on-site detection of drugs in sewage, on-site detection of organic matters in aqueous phase samples in environmental detection, on-site detection of organic matters in aqueous phase samples in food detection, and the like, the components in the liquid phase samples are complex, so that the analysis and the determination can be performed only after pretreatment, and the specific purpose is to concentrate trace detected components and improve the sensitivity of the method; removing the matrix and other interfering substances in the sample; the mass and the volume of the sample are concentrated, so that the transportation and the preservation are convenient, the stability of the sample is improved, and the like.
In the prior art, for detection and analysis of liquid phase samples, the traditional pretreatment technology includes a solid phase extraction technology, a liquid-liquid extraction technology and the like. The existing pretreatment technologies have the defects of complex operation, long extraction time, high cost and the like, and can be completed only in specific environments and instruments such as laboratories.
In addition, in the detection analysis of the liquid phase sample in the prior art, especially in the field detection, the defect that the timeliness of the detection result is poor due to the overlong detection time exists. Especially in drug case investigation and investigation, the requirement on timeliness cannot be met.
Disclosure of Invention
In order to overcome the defects of the prior art, the application aims to provide the liquid phase detection sample enrichment pretreatment method which has the advantages of simple operation and low cost and can solve the problem of poor timeliness of detection results caused by overlong detection time in field detection.
In order to achieve the purpose of the application, the technical scheme adopted by the application is as follows:
the application provides a pretreatment method for enrichment of a liquid phase detection sample, which comprises the following steps:
sample enrichment: enriching the components to be detected of the sample by using an enrichment device or an extraction device, and extracting by using alcohol substances to obtain alcohol extract;
ultrasonic extraction and vacuum concentration synchronous treatment: placing the alcohol extract in a test tube, connecting the test tube with a vacuum instrument, placing the test tube in an ultrasonic instrument, and starting the ultrasonic instrument and the vacuum instrument until alcohol substances in the test tube volatilize to dryness to obtain components to be tested of the test sample;
and (3) re-dissolving and vortex treatment: taking out the test tube, adding an extracting solution to re-dissolve components to be tested of a sample of the test tube, and placing the test tube on a vortex instrument for oscillation treatment to obtain a liquid to be tested;
heating and hatching: and placing the detection reagent card on a heating instrument, dripping the to-be-detected liquid into the detection reagent card, and heating and hatching to obtain a to-be-detected sample which can be used for detection of the detection instrument.
The method comprises the steps of enriching and extracting a sample to obtain an alcohol extract, vacuumizing the alcohol extract while carrying out ultrasound to volatilize alcohol substances to obtain a component to be tested of the sample, re-dissolving the component to be tested of the sample by using the extract, carrying out oscillation treatment on the component to be tested of the sample by using a vortex instrument to obtain a liquid to be tested, finally dripping the liquid to be tested into a test reagent card, and carrying out heating hatching to complete the pretreatment of enriching the liquid phase test sample. The pretreatment method for enrichment of the liquid phase detection sample has the advantages of simple operation, short extraction time, low cost and the like, and can be completed without specific environments and instruments such as a laboratory and the like. In addition, in some field detection, especially in drug case investigation, can shorten the detection duration greatly, and then have the advantage that testing result timeliness is good.
Further, the liquid phase detection sample enrichment pretreatment method is to utilize a liquid phase detection sample enrichment pretreatment device to carry out treatment operation, wherein the liquid phase detection sample enrichment pretreatment device comprises an ultrasonic instrument, a vacuum instrument, a vortex instrument and a heating instrument which are arranged in a device main body.
Because the enrichment pretreatment device for the liquid phase detection sample integrates an ultrasonic instrument, a vacuum instrument, a vortex instrument and a heating instrument, the enrichment pretreatment device can be directly used for enrichment pretreatment operation of the liquid phase sample in field detection, and therefore the enrichment pretreatment device has the advantages of being simple in operation, capable of greatly shortening detection time length and further good in timeliness of detection results.
Further, the liquid phase detection sample enrichment pretreatment device further comprises a fan, wherein the fan is arranged on one side of the ultrasonic instrument and used for cooling the ultrasonic instrument. In the process of carrying out ultrasound on the alcohol extract by the ultrasonic instrument, the heat of the alcohol extract can be increased due to ultrasonic vibration, and if the temperature is too high, the stability of a component to be detected in the alcohol extract can be affected, so that the final sample detection result can be affected. Therefore, in the process of carrying out ultrasound by the ultrasound instrument, the fan is started to drive air to circulate so as to rapidly take away the heat generated by the ultrasound instrument, and further the influence of the too high temperature of the alcohol extract on the detection result of the sample is avoided.
Further, the sample enrichment step is: placing a metal net with enrichment balls into a sample, enriching the components to be detected of the sample, taking out the enrichment balls, transferring the enrichment balls into a test tube, and adding alcohol substances for extraction to obtain an alcohol extract. Wherein the test tube may be a vacuum tube.
Wherein the sample enrichment step is performed on an off-the-shelf sample. Enrichment spheres are a class of microspheres that are capable of separating adsorbed organics from the liquid phase. After the enrichment ball is placed in the sample, the component to be detected in the sample is adsorbed. After the enrichment ball finishes the adsorption of the components to be detected, the enrichment ball is taken out, an alcohol substance is added into the enrichment ball, the components to be detected adsorbed by the enrichment ball are extracted by the alcohol substance, and an alcohol extract is obtained, namely, the components to be detected in the sample are dissolved into the alcohol substance to form the alcohol extract.
Further, the sample enrichment step is: and placing a liquid phase sample collected on site in a container, sequentially connecting the container with an SPE (solid phase extraction) column, a filter flask and a vacuum instrument, starting the vacuum instrument to enable the liquid phase sample in the container to flow through the SPE column, taking down the SPE column, and adding alcohol substances into the SPE column to elute components to be detected of the sample adsorbed in the SPE column to obtain an alcohol extract.
Wherein, the sample enrichment step is an operation of forming a sample and enriching for a field collected sample. The liquid phase sample collected on site is placed in a container, a container bottle can be used, the container bottle is sequentially connected with an SPE column, a filter bottle and a vacuum instrument, and through vacuumizing operation, the components to be tested in the liquid phase sample are finally adsorbed to the SPE column, then alcohol substances are utilized for eluting and extracting, and finally the components to be tested in the sample are extracted by the alcohol substances to form alcohol extract.
Further, the alcohol substance comprises at least one of methanol, ethanol or propanol.
Wherein, the methanol, the ethanol or the propanol has better solubility to organic matters, and can extract the components to be detected of the sample from the enrichment ball or the SPE column. In addition, the methanol, the ethanol or the propanol also has better volatilization intensity, can completely volatilize in the vacuumizing operation, and further the rest components to be detected are used for the subsequent pretreatment operation. In the actual extraction operation, methanol is a common alcohol substance.
Further, in the sample enrichment, the mass ratio of the alcohol substances to the sample is 3-10:1; the alcohol substance is used for extracting the component to be detected in the sample, and the proper mass ratio does not influence the sufficiency of extraction and does not waste materials. And/or
In the ultrasonic extraction and vacuum concentration synchronous treatment step, the time for starting the ultrasonic instrument and the vacuum instrument is 15-20 min.
Further, in the step of redissolution and vortex treatment, the mass ratio of the extracting solution to the components to be detected of the sample is 2-10:1; the extracting solution is used for redissolving the components to be detected of the sample, and the components to be detected of the sample and the extracting solution are uniformly mixed through vortex treatment. The proper mass ratio does not affect the sufficiency of dissolution nor waste materials.
And/or
Further, the test tube is placed on a vortex machine for oscillation treatment for 5 s-10 s. Wherein, the vibration treatment for 5s to 10s on the vortex instrument can well ensure that the components to be measured of the sample and the extracting solution are uniformly mixed.
Further, in the step of redissolution and vortex treatment, the extracting solution comprises the following components in concentration:
wherein, potassium dihydrogen phosphate and dipotassium hydrogen phosphate form phosphate buffer salt together so as to provide an environment suitable for the reaction of the detection reagent. The sodium dodecyl benzene sulfonate can enable the extracting solution to more effectively and fully absorb and dissolve components to be detected of the sample, so that the dissolving and adsorbing amount is improved, the speed of detection reaction is improved, and the detection efficiency and the accuracy are improved. The ethylenediamine tetraacetic acid is used for eliminating heavy metal ions possibly existing in the extracting solution, so that the interference of the heavy metal ions on components to be detected of the sample is reduced, and the effect of improving the detection accuracy is achieved. Sodium azide is used as a preservative and can enhance the quality guarantee effect of the extracting solution.
Further, in the heating and hatching step, the heating temperature of the heater is 29-35 ℃, and the heating and hatching time is 5-8 min. The heating temperature is moderate, the temperature requirement of the detector on the liquid to be detected in the detection reagent card can be matched, the detection sensitivity can be improved, and the stability of the liquid to be detected can not be affected by the temperature.
In addition, in the actual detection process, after the heating and hatching steps are completed, a detection reagent card in which the liquid to be detected is dripped can be inserted into a slot of the detector, and detection data results can be read on a screen of the detector. When drugs are detected, the detector is a full biological sample drug detector.
Compared with the prior art, the application has the beneficial effects that:
(1) According to the liquid phase detection sample enrichment pretreatment method, firstly, an alcohol extracting solution is obtained by enriching and extracting a sample, then the alcohol extracting solution is vacuumized while ultrasonic treatment is carried out to volatilize alcohol substances to obtain a sample component to be detected, the extracting solution is utilized to redissolve the sample component to be detected, the vibration treatment on a vortex meter is utilized to obtain a liquid to be detected, finally, the liquid to be detected is dripped into a detection reagent card, and heating hatching is carried out, so that the liquid phase detection sample enrichment pretreatment is completed. The pretreatment method for enrichment of the liquid phase detection sample has the advantages of simple operation, short extraction time, low cost and the like, and can be completed without specific environments and instruments such as a laboratory and the like. In addition, in some field detection, especially in drug case investigation, can shorten the detection duration greatly, and then have the advantage that testing result timeliness is good.
(2) The liquid phase detection sample enrichment pretreatment method of the application utilizes a liquid phase detection sample enrichment pretreatment device to carry out treatment operation, and the liquid phase detection sample enrichment pretreatment device comprises an ultrasonic instrument, a vacuum instrument, a vortex instrument and a heating instrument which are arranged in a device main body. Because the enrichment pretreatment device for the liquid phase detection sample integrates an ultrasonic instrument, a vacuum instrument, a vortex instrument and a heating instrument, the enrichment pretreatment device can be directly used for enrichment pretreatment operation of the liquid phase sample in field detection, and therefore the enrichment pretreatment device has the advantages of being simple in operation, capable of greatly shortening detection time length and further good in timeliness of detection results.
(3) The enrichment pretreatment method of the liquid phase detection sample is suitable for carrying out enrichment pretreatment operation on the existing liquid phase sample and then carrying out detection analysis; the sample enrichment pretreatment device is also suitable for forming samples and enriching the samples on site, particularly for utilizing a liquid phase detection sample enrichment pretreatment device integrating an ultrasonic instrument, a vacuum instrument, a vortex instrument and a heating instrument, is very convenient for collecting the samples on site to form the samples and enriching, namely, carrying out series of pretreatment operations, and is very suitable for being used in site detection, particularly for site detection in drug case investigation and investigation.
(4) The pretreatment method for enrichment of the liquid phase detection sample has the characteristics of simple operation method, high treatment efficiency and high detection accuracy.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects to be solved more clear, the application is further described in detail below with reference to the embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the application.
The terminology used in the embodiments of the application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used in this specification, the singular forms "a", "an", and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
Wherein, the SPE column refers to an extraction column.
In the embodiment of the application, the liquid phase detection sample enrichment pretreatment method comprises the following steps:
sample enrichment: enriching the components to be detected of the sample by using an enrichment device or an extraction device, and extracting by using alcohol substances to obtain alcohol extract;
ultrasonic extraction and vacuum concentration synchronous treatment: placing the alcohol extract in a test tube, connecting the test tube with a vacuum instrument, placing the test tube in an ultrasonic instrument, and starting the ultrasonic instrument and the vacuum instrument until alcohol substances in the test tube volatilize to dryness to obtain components to be tested of the test sample;
and (3) re-dissolving and vortex treatment: taking out the test tube, adding an extracting solution to re-dissolve components to be tested of a sample of the test tube, and placing the test tube on a vortex instrument for oscillation treatment to obtain a liquid to be tested;
heating and hatching: and placing the detection reagent card on a heating instrument, dripping the to-be-detected liquid into the detection reagent card, and heating and hatching to obtain a to-be-detected sample which can be used for detection of the detection instrument.
The method comprises the steps of enriching and extracting a sample to obtain an alcohol extract, vacuumizing the alcohol extract while performing ultrasonic treatment to volatilize alcohol substances to obtain a component to be tested of the sample, re-dissolving the component to be tested of the sample by using the extract, performing oscillation treatment on the component to be tested of the sample by using a vortex meter to obtain a liquid to be tested, finally dripping the liquid to be tested into a test reagent card, and performing heating hatching to complete the pretreatment of enriching the liquid phase test sample. The pretreatment method for enrichment of the liquid phase detection sample has the advantages of simple operation, short extraction time, low cost and the like, and can be completed without specific environments and instruments such as a laboratory and the like. In addition, in some field detection, especially in drug case investigation, can shorten the detection duration greatly, and then have the advantage that testing result timeliness is good.
In some embodiments, the liquid phase detection sample enrichment pretreatment method utilizes a liquid phase detection sample enrichment pretreatment device to carry out treatment operation, wherein the liquid phase detection sample enrichment pretreatment device comprises an ultrasonic instrument, a vacuum instrument, a vortex instrument and a heating instrument which are arranged in a device main body.
Because the enrichment pretreatment device for the liquid phase detection sample integrates an ultrasonic instrument, a vacuum instrument, a vortex instrument and a heating instrument, the enrichment pretreatment device can be directly used for enrichment pretreatment operation of the liquid phase sample in field detection, and therefore the enrichment pretreatment device has the advantages of being simple in operation, capable of greatly shortening detection time length and further good in timeliness of detection results.
In some embodiments, the liquid phase detection sample enrichment pretreatment device further comprises a fan, wherein the fan is arranged on one side of the ultrasonic instrument and used for cooling the ultrasonic instrument. In the process of carrying out ultrasound on the alcohol extract by the ultrasonic instrument, the heat of the alcohol extract can be increased due to ultrasonic vibration, and if the temperature is too high, the stability of a component to be detected in the alcohol extract can be affected, so that the final sample detection result can be affected. Therefore, in the process of carrying out ultrasound by the ultrasound instrument, the fan is started to drive air to circulate so as to rapidly take away the heat generated by the ultrasound instrument, and further the influence of the too high temperature of the alcohol extract on the detection result of the sample is avoided.
In some embodiments, the sample enrichment step is: placing a metal net with enrichment balls into a sample, enriching the components to be detected of the sample, taking out the enrichment balls, transferring the enrichment balls into a test tube, and adding alcohol substances for extraction to obtain an alcohol extract. Wherein, the test tube can be a vacuum tube.
Wherein the sample enrichment step is performed on an off-the-shelf sample. Enrichment spheres are a class of microspheres that are capable of separating adsorbed organics from a gas or liquid phase. After the enrichment ball is placed in the sample, the enrichment ball is promoted to adsorb the components to be detected in the sample through ultrasonic vibration. After the enrichment ball finishes the adsorption of the components to be detected, the enrichment ball is taken out, an alcohol substance is added into the enrichment ball, the components to be detected adsorbed by the enrichment ball are extracted by the alcohol substance, and an alcohol extract is obtained, namely, the components to be detected in the sample are dissolved into the alcohol substance to form the alcohol extract.
In some embodiments, the sample enrichment step is: and placing a liquid phase sample collected on site in a container, sequentially connecting the container with an SPE (solid phase extraction) column, a filter flask and a vacuum instrument, starting the vacuum instrument to enable the liquid phase sample in the container to flow through the SPE column, taking down the SPE column, and adding alcohol substances into the SPE column to elute components to be detected of the sample adsorbed in the SPE column, thereby obtaining an alcohol extract.
Wherein, the sample enrichment step is an operation of forming a sample and enriching for a field collected sample. The liquid phase sample collected on site is placed in a container, a container bottle can be used, the container bottle is sequentially connected with an SPE column, a filter bottle and a vacuum instrument, and through vacuumizing operation, the components to be tested in the liquid phase sample are finally adsorbed to the SPE column, then alcohol substances are utilized for eluting and extracting, and finally the components to be tested in the sample are extracted by the alcohol substances to form alcohol extract.
In some embodiments, the alcohol comprises at least one of methanol, ethanol, or propanol.
Wherein, the methanol, the ethanol or the propanol has better solubility to organic matters, and can extract the components to be detected of the sample from the enrichment ball or the SPE column. In addition, the methanol, the ethanol or the propanol also has better volatilization intensity, can completely volatilize in the vacuumizing operation, and further the rest components to be detected are used for the subsequent pretreatment operation. In the actual extraction operation, methanol is a common alcohol substance.
In some embodiments, the mass ratio of alcohol species to sample is 3-10:1 in the sample enrichment; the alcohol substance is used for extracting the component to be detected in the sample, and the proper mass ratio does not influence the sufficiency of extraction and does not waste materials.
In some embodiments, in the step of synchronous treatment of ultrasonic extraction and vacuum concentration, the time for starting the ultrasonic instrument and the vacuum instrument is 15-20 min.
In some embodiments, in the steps of redissolution and vortex treatment, the mass ratio of the extracting solution to the component to be measured of the sample is 2-10:1; the extracting solution is used for redissolving the components to be detected of the sample, and the components to be detected of the sample and the extracting solution are uniformly mixed through vortex treatment. The proper mass ratio does not affect the sufficiency of dissolution nor waste materials.
In some embodiments, the test tube is placed on a vortexing apparatus for a period of 5s to 10s with shaking. Wherein, the vibration treatment for 5s to 10s on the vortex instrument can well ensure that the components to be measured of the sample and the extracting solution are uniformly mixed.
In some embodiments, in the reconstitution and vortexing steps, the extract comprises the following concentrations of components:
wherein, potassium dihydrogen phosphate and dipotassium hydrogen phosphate form phosphate buffer salt together so as to provide an environment suitable for the reaction of the detection reagent. The sodium dodecyl benzene sulfonate can enable the extracting solution to more effectively and fully absorb and dissolve components to be detected of the sample, so that the dissolving and adsorbing amount is improved, the speed of detection reaction is improved, and the detection efficiency and the accuracy are improved. The ethylenediamine tetraacetic acid is used for eliminating heavy metal ions possibly existing in the extracting solution, so that the interference of the heavy metal ions on components to be detected of the sample is reduced, and the effect of improving the detection accuracy is achieved. Sodium azide is used as a preservative and can enhance the quality guarantee effect of the extracting solution.
In some embodiments, in the heating and hatching step, the heating temperature of the heater is 29-35 ℃ and the heating and hatching time is 5-8 min. The heating temperature is moderate, the temperature requirement of the detector on the liquid to be detected in the detection reagent card can be matched, the detection sensitivity can be improved, and the stability of the liquid to be detected can not be affected by the temperature.
In addition, in the actual detection process, after the heating and hatching steps are completed, a detection reagent card in which the liquid to be detected is dripped can be inserted into a slot of the detector, and detection data results can be read on a screen of the detector. When drugs are detected, the detector is a full biological sample drug detector.
The following description is made with reference to specific embodiments.
Example 1
The pretreatment method for enrichment of the liquid phase detection sample comprises the following steps:
sample enrichment: enriching the components to be detected of the sample by using an enrichment device or an extraction device, and extracting by using alcohol substances to obtain alcohol extract;
ultrasonic extraction and vacuum concentration synchronous treatment: placing the alcohol extract in a test tube, connecting the test tube with a vacuum instrument, placing the test tube in an ultrasonic instrument, and starting the ultrasonic instrument and the vacuum instrument until alcohol substances in the test tube volatilize to dryness to obtain components to be tested of the test sample;
and (3) re-dissolving and vortex treatment: taking out the test tube, adding an extracting solution to re-dissolve components to be tested of a sample of the test tube, and placing the test tube on a vortex instrument for oscillation treatment to obtain a liquid to be tested;
heating and hatching: and placing the detection reagent card on a heating instrument, dripping the to-be-detected liquid into the detection reagent card, and heating and hatching to obtain a to-be-detected sample which can be used for detection of the detection instrument.
In this embodiment, the liquid phase detection sample enrichment pretreatment method performs a treatment operation by using a liquid phase detection sample enrichment pretreatment device, where the liquid phase detection sample enrichment pretreatment device includes an ultrasonic instrument, a vacuum instrument, a vortex instrument, and a heating instrument that are disposed in a device body.
In this embodiment, the liquid phase detection sample enrichment pretreatment device further includes a fan, where the fan is disposed on one side of the ultrasonic apparatus and is used to cool the ultrasonic apparatus.
In this example, the sample enrichment step is: placing a metal net with enrichment balls into a sample, enriching the components to be detected of the sample, taking out the enrichment balls, transferring the enrichment balls into a test tube, and adding alcohol substances for extraction to obtain an alcohol extract. Wherein, the test tube can be a vacuum tube.
In this embodiment, the alcohol includes methanol.
In this example, the mass ratio of the alcohol substance to the sample was 5:1.
In the embodiment, in the step of synchronous treatment of ultrasonic extraction and vacuum concentration, the time for starting the ultrasonic instrument and the vacuum instrument is 18 minutes.
In the embodiment, in the steps of redissolution and vortex treatment, the mass ratio of the extracting solution to the components to be detected of the sample is 5:1.
In this example, the test tube was placed on a vortexing apparatus for 8 seconds with shaking.
In this embodiment, in the steps of reconstitution and vortexing, the extract comprises the following concentrations of components:
in this embodiment, in the heating and hatching step, the heating temperature of the heater is 33 ℃, and the heating and hatching time is 6min.
Example 2
The pretreatment method for enrichment of the liquid phase detection sample comprises the following steps:
sample enrichment: enriching the components to be detected of the sample by using an enrichment device or an extraction device, and extracting by using alcohol substances to obtain alcohol extract;
ultrasonic extraction and vacuum concentration synchronous treatment: placing the alcohol extract in a test tube, connecting the test tube with a vacuum instrument, placing the test tube in an ultrasonic instrument, and starting the ultrasonic instrument and the vacuum instrument until alcohol substances in the test tube volatilize to dryness to obtain components to be tested of the test sample;
and (3) re-dissolving and vortex treatment: taking out the test tube, adding an extracting solution to re-dissolve components to be tested of a sample of the test tube, and placing the test tube on a vortex instrument for oscillation treatment to obtain a liquid to be tested;
heating and hatching: and placing the detection reagent card on a heating instrument, dripping the to-be-detected liquid into the detection reagent card, and heating and hatching to obtain a to-be-detected sample which can be used for detection of the detection instrument.
In this embodiment, the liquid phase detection sample enrichment pretreatment method performs a treatment operation by using a liquid phase detection sample enrichment pretreatment device, where the liquid phase detection sample enrichment pretreatment device includes an ultrasonic instrument, a vacuum instrument, a vortex instrument, and a heating instrument that are disposed in a device body.
In this embodiment, the liquid phase detection sample enrichment pretreatment device further includes a fan, where the fan is disposed on one side of the ultrasonic apparatus and is used to cool the ultrasonic apparatus.
In this example, the sample enrichment step is: and placing a liquid phase sample collected on site into a container, sequentially connecting the container with an SPE (solid phase extraction) column, a filter flask and a vacuum instrument, starting the vacuum instrument to enable the liquid phase sample in the container to flow through the SPE column, taking down the SPE column, and adding alcohol substances into the SPE column to elute components to be detected of the sample adsorbed in the SPE column to obtain an alcohol extract.
In this embodiment, the alcohol includes ethanol.
In this example, the mass ratio of the alcohol substance to the sample was 3:1.
In the embodiment, in the step of synchronous treatment of ultrasonic extraction and vacuum concentration, the time for starting the ultrasonic instrument and the vacuum instrument is 15min.
In the embodiment, in the steps of redissolution and vortex treatment, the mass ratio of the extracting solution to the components to be detected of the sample is 2:1.
In this example, the test tube was placed on a vortexing apparatus for a period of 5s with shaking.
In this embodiment, in the steps of reconstitution and vortexing, the extract comprises the following concentrations of components:
in this embodiment, in the heating and hatching step, the heating temperature of the heater is 29 ℃, and the heating and hatching time is 8min.
Example 3
The pretreatment method for enrichment of the liquid phase detection sample comprises the following steps:
sample enrichment: enriching the components to be detected of the sample by using an enrichment device or an extraction device, and extracting by using alcohol substances to obtain alcohol extract;
ultrasonic extraction and vacuum concentration synchronous treatment: placing the alcohol extract in a test tube, connecting the test tube with a vacuum instrument, placing the test tube in an ultrasonic instrument, and starting the ultrasonic instrument and the vacuum instrument until alcohol substances in the test tube volatilize to dryness to obtain components to be tested of the test sample;
and (3) re-dissolving and vortex treatment: taking out the test tube, adding an extracting solution to re-dissolve components to be tested of a sample of the test tube, and placing the test tube on a vortex instrument for oscillation treatment to obtain a liquid to be tested;
heating and hatching: and placing the detection reagent card on a heating instrument, dripping the to-be-detected liquid into the detection reagent card, and heating and hatching to obtain a to-be-detected sample which can be used for detection of the detection instrument.
In this embodiment, the liquid phase detection sample enrichment pretreatment method performs a treatment operation by using a liquid phase detection sample enrichment pretreatment device, where the liquid phase detection sample enrichment pretreatment device includes an ultrasonic instrument, a vacuum instrument, a vortex instrument, and a heating instrument that are disposed in a device body.
In this embodiment, the liquid phase detection sample enrichment pretreatment device further includes a fan, where the fan is disposed on one side of the ultrasonic apparatus and is used to cool the ultrasonic apparatus.
In this example, the sample enrichment step is: placing a metal net with enrichment balls into a sample, enriching the components to be detected of the sample, taking out the enrichment balls, transferring the enrichment balls into a test tube, and adding alcohol substances for extraction to obtain an alcohol extract. Wherein, the test tube can be a vacuum tube.
In this embodiment, the alcohol includes propanol.
In this example, the mass ratio of the alcohol substance to the sample was 10:1.
In this embodiment, in the step of synchronous processing of ultrasonic extraction and vacuum concentration, the time for starting the ultrasonic apparatus and the vacuum apparatus is 20 minutes.
In the embodiment, in the steps of redissolution and vortex treatment, the mass ratio of the extracting solution to the components to be detected of the sample is 10:1.
In this example, the test tube was placed on a vortexing apparatus for a period of 10s with shaking.
In this embodiment, in the steps of reconstitution and vortexing, the extract comprises the following concentrations of components:
in this embodiment, in the heating and hatching step, the heating temperature of the heater is 35 ℃, and the heating and hatching time is 5min.
Example 4
The pretreatment method for enrichment of the liquid phase detection sample comprises the following steps:
sample enrichment: enriching the components to be detected of the sample by using an enrichment device or an extraction device, and extracting by using alcohol substances to obtain alcohol extract;
ultrasonic extraction and vacuum concentration synchronous treatment: placing the alcohol extract in a test tube, connecting the test tube with a vacuum instrument, placing the test tube in an ultrasonic instrument, and starting the ultrasonic instrument and the vacuum instrument until alcohol substances in the test tube volatilize to dryness to obtain components to be tested of the test sample;
and (3) re-dissolving and vortex treatment: taking out the test tube, adding an extracting solution to re-dissolve components to be tested of a sample of the test tube, and placing the test tube on a vortex instrument for oscillation treatment to obtain a liquid to be tested;
heating and hatching: and placing the detection reagent card on a heating instrument, dripping the to-be-detected liquid into the detection reagent card, and heating and hatching to obtain a to-be-detected sample which can be used for detection of the detection instrument.
In this embodiment, the liquid phase detection sample enrichment pretreatment method performs a treatment operation by using a liquid phase detection sample enrichment pretreatment device, where the liquid phase detection sample enrichment pretreatment device includes an ultrasonic instrument, a vacuum instrument, a vortex instrument, and a heating instrument that are disposed in a device body.
In this embodiment, the liquid phase detection sample enrichment pretreatment device further includes a fan, where the fan is disposed on one side of the ultrasonic apparatus and is used to cool the ultrasonic apparatus.
In this example, the sample enrichment step is: and placing a liquid phase sample collected on site in a container, sequentially connecting the container with an SPE (solid phase extraction) column, a filter flask and a vacuum instrument, starting the vacuum instrument to enable the liquid phase sample in the container to flow through the SPE column, taking down the SPE column, and adding alcohol substances into the SPE column to elute components to be detected of the sample adsorbed in the SPE column to obtain an alcohol extract.
In this embodiment, the alcohol includes a mixture of methanol and ethanol.
In this example, the mass ratio of the alcohol substance to the sample was 4:1.
In the embodiment, in the step of synchronous treatment of ultrasonic extraction and vacuum concentration, the time for starting the ultrasonic instrument and the vacuum instrument is 16min.
In the embodiment, in the steps of redissolution and vortex treatment, the mass ratio of the extracting solution to the components to be detected of the sample is 3:1.
In this example, the test tube was placed on a vortexing apparatus for a period of 6s with shaking.
In this embodiment, in the steps of reconstitution and vortexing, the extract comprises the following concentrations of components:
in this embodiment, in the heating and hatching step, the heating temperature of the heater is 30 ℃, and the heating and hatching time is 7.5min.
Example 5
The pretreatment method for enrichment of the liquid phase detection sample comprises the following steps:
sample enrichment: enriching the components to be detected of the sample by using an enrichment device or an extraction device, and extracting by using alcohol substances to obtain alcohol extract;
ultrasonic extraction and vacuum concentration synchronous treatment: placing the alcohol extract in a test tube, connecting the test tube with a vacuum instrument, placing the test tube in an ultrasonic instrument, and starting the ultrasonic instrument and the vacuum instrument until alcohol substances in the test tube volatilize to dryness to obtain components to be tested of the test sample;
and (3) re-dissolving and vortex treatment: taking out the test tube, adding an extracting solution to re-dissolve components to be tested of a sample of the test tube, and placing the test tube on a vortex instrument for oscillation treatment to obtain a liquid to be tested;
heating and hatching: and placing the detection reagent card on a heating instrument, dripping the to-be-detected liquid into the detection reagent card, and heating and hatching to obtain a to-be-detected sample which can be used for detection of the detection instrument.
In this embodiment, the liquid phase detection sample enrichment pretreatment method performs a treatment operation by using a liquid phase detection sample enrichment pretreatment device, where the liquid phase detection sample enrichment pretreatment device includes an ultrasonic instrument, a vacuum instrument, a vortex instrument, and a heating instrument that are disposed in a device body.
In this embodiment, the liquid phase detection sample enrichment pretreatment device further includes a fan, where the fan is disposed on one side of the ultrasonic apparatus and is used to cool the ultrasonic apparatus.
In this example, the sample enrichment step is: placing a metal net with enrichment balls into a sample, enriching the components to be detected of the sample, taking out the enrichment balls, transferring the enrichment balls into a test tube, and adding alcohol substances for extraction to obtain an alcohol extract. Wherein, the test tube can be a vacuum tube.
In this embodiment, the alcohol includes a mixture of methanol and propanol.
In this example, the mass ratio of the alcohol substance to the sample was 9:1.
In this embodiment, in the step of synchronous processing of ultrasonic extraction and vacuum concentration, the time for starting the ultrasonic apparatus and the vacuum apparatus is 19min.
In the embodiment, in the steps of redissolution and vortex treatment, the mass ratio of the extracting solution to the components to be detected of the sample is 9:1.
In this example, the test tube was placed on a vortexing apparatus for a period of 9s with shaking.
In this embodiment, in the steps of reconstitution and vortexing, the extract comprises the following concentrations of components:
in this embodiment, in the heating and hatching step, the heating temperature of the heater is 34 ℃, and the heating and hatching time is 5.5min.
Example 6
The pretreatment method for enrichment of the liquid phase detection sample comprises the following steps:
sample enrichment: enriching the components to be detected of the sample by using an enrichment device or an extraction device, and extracting by using alcohol substances to obtain alcohol extract;
ultrasonic extraction and vacuum concentration synchronous treatment: placing the alcohol extract in a test tube, connecting the test tube with a vacuum instrument, placing the test tube in an ultrasonic instrument, and starting the ultrasonic instrument and the vacuum instrument until alcohol substances in the test tube volatilize to dryness to obtain components to be tested of the test sample;
and (3) re-dissolving and vortex treatment: taking out the test tube, adding an extracting solution to re-dissolve components to be tested of a sample of the test tube, and placing the test tube on a vortex instrument for oscillation treatment to obtain a liquid to be tested;
heating and hatching: and placing the detection reagent card on a heating instrument, dripping the to-be-detected liquid into the detection reagent card, and heating and hatching to obtain a to-be-detected sample which can be used for detection of the detection instrument.
In this embodiment, the liquid phase detection sample enrichment pretreatment method performs a treatment operation by using a liquid phase detection sample enrichment pretreatment device, where the liquid phase detection sample enrichment pretreatment device includes an ultrasonic instrument, a vacuum instrument, a vortex instrument, and a heating instrument that are disposed in a device body.
In this embodiment, the liquid phase detection sample enrichment pretreatment device further includes a fan, where the fan is disposed on one side of the ultrasonic apparatus and is used to cool the ultrasonic apparatus.
In this example, the sample enrichment step is: and placing a liquid phase sample collected on site in a container, sequentially connecting the container with an SPE (solid phase extraction) column, a filter flask and a vacuum instrument, starting the vacuum instrument to enable the liquid phase sample in the container to flow through the SPE column, taking down the SPE column, and adding alcohol substances into the SPE column to elute components to be detected of the sample adsorbed in the SPE column to obtain an alcohol extract.
In this embodiment, the alcohol comprises a combination of ethanol and propanol.
In this example, the mass ratio of the alcohol substance to the sample was 6:1.
In the embodiment, in the step of synchronous treatment of ultrasonic extraction and vacuum concentration, the time for starting the ultrasonic instrument and the vacuum instrument is 17min.
In the embodiment, in the steps of redissolution and vortex treatment, the mass ratio of the extracting solution to the components to be detected of the sample is 6:1.
In this example, the test tube was placed on a vortexing apparatus for a period of 7s with shaking.
In this embodiment, in the steps of reconstitution and vortexing, the extract comprises the following concentrations of components:
in this embodiment, in the heating and hatching step, the heating temperature of the heater is 31 ℃, and the heating and hatching time is 7min.
The foregoing description of the preferred embodiments of the application is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the application.
Claims (10)
1. The pretreatment method for enrichment of the liquid phase detection sample is characterized by comprising the following steps:
sample enrichment: enriching the components to be detected of the sample by using an enrichment device or an extraction device, and extracting by using alcohol substances to obtain alcohol extract;
ultrasonic extraction and vacuum concentration synchronous treatment: placing the alcohol extract in a test tube, connecting the test tube with a vacuum instrument, placing the test tube in an ultrasonic instrument, and starting the ultrasonic instrument and the vacuum instrument until alcohol substances in the test tube volatilize to dryness to obtain components to be tested of the test sample;
and (3) re-dissolving and vortex treatment: taking out the test tube, adding an extracting solution to re-dissolve components to be tested of a sample of the test tube, and placing the test tube on a vortex instrument for oscillation treatment to obtain a liquid to be tested;
heating and hatching: and placing the detection reagent card on a heating instrument, dripping the to-be-detected liquid into the detection reagent card, and heating and hatching to obtain a to-be-detected sample which can be used for detection of the detection instrument.
2. The method for pretreatment of enrichment of liquid phase detection sample according to claim 1, wherein the pretreatment device for enrichment of liquid phase detection sample is used for the treatment operation, and the pretreatment device for enrichment of liquid phase detection sample comprises an ultrasonic instrument, a vacuum instrument, a vortex instrument and a heating instrument which are arranged in the device body.
3. The method according to claim 2, wherein the pretreatment device for enrichment of liquid phase detection sample further comprises a fan, and the fan is disposed at one side of the ultrasonic instrument and is used for cooling the ultrasonic instrument.
4. The method for pretreatment of enrichment of liquid phase detection sample according to claim 1, wherein said sample enrichment step is: placing a metal net with enrichment balls into a sample, enriching the components to be detected of the sample, taking out the enrichment balls, transferring the enrichment balls into a test tube, and adding alcohol substances for extraction to obtain an alcohol extract.
5. The method for pretreatment of enrichment of liquid phase detection sample according to claim 1, wherein said sample enrichment step is: and placing a liquid phase sample collected on site in a container, sequentially connecting the container with an SPE (solid phase extraction) column, a filter flask and a vacuum instrument, starting the vacuum instrument to enable the liquid phase sample in the container to flow through the SPE column, taking down the SPE column, and adding alcohol substances into the SPE column to elute components to be detected of the sample adsorbed in the SPE column to obtain an alcohol extract.
6. The method for pretreatment of enrichment of liquid phase detection samples according to any of claims 1, 4 and 5, wherein the alcohol comprises at least one of methanol, ethanol or propanol.
7. The pretreatment method for enrichment of liquid phase detection sample according to claim 1, wherein the mass ratio of said alcohol substance to said sample in said sample enrichment is 3-10:1; and/or
In the ultrasonic extraction and vacuum concentration synchronous treatment step, the time for starting the ultrasonic instrument and the vacuum instrument is 15-20 min.
8. The method for pretreatment of enrichment of liquid phase detection sample according to claim 1, wherein in the step of redissolution and vortex treatment, the mass ratio of the extract to the component to be detected of the sample is 2-10:1; and/or
The test tube is placed on a vortex meter for oscillation treatment for 5 s-10 s.
9. The method for pretreatment of enrichment of liquid phase detection sample according to claim 1, wherein in the step of redissolution and vortexing, the extract comprises the following components in concentration:
potassium dihydrogen phosphate 0.01mol/L to 0.1mol/L
Dipotassium hydrogen phosphate 0.01 mol/L-0.1 mol/L
Sodium dodecyl benzene sulfonate 0.01 mol/L-0.1 mol/L
0.01mol/L to 0.1mol/L of ethylenediamine tetraacetic acid
Sodium azide of 0.01mol/L to 0.1mol/L
The solvent is water.
10. The pretreatment method for enrichment of liquid phase detection samples according to claim 1, wherein in the heating and incubation step, the heating temperature of the heater is 29-35 ℃, and the heating and incubation time is 5-8 min.
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