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43 results about "Gc nci ms" patented technology
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Pretreatment method of polybrominated diphenyl ethers in environment solid matrix
ActiveCN104713964AImplement batch processingMicrowave extraction method is simpleComponent separationPretreatment methodFiltration
The invention relates to a pretreatment method of polybrominated diphenyl ethers in an environment solid matrix, which is characterized in that a combined technology of microwave auxiliary extraction and solid phase extraction is used for processing solid matrix PBDEs such as soil and deposits. The method comprises the following steps: 1)drying and crushing a sample; 2)performing microwave auxiliary extraction: weighing a soil deposit sample to be processed, weighing a certain amount of extraction solvent, using a microwave digestion / extraction instrument for microwave auxiliary extraction; 3)performing solid-liquid separation; 4)solid phase purification and purification by a small column: performing rotary evaporation on the extract to about 1ml, through solid phase extraction and purification by the small column; and 5)subsequent processing: performing nitrogen blowing on an eluate to a dry state, metering volume on the solvent, after membrane filtration, and using GC-NCI-MS for analysis. According to the invention, pre-treatment time of the sample is short, decomposition of unstable substances such as PBDEs can be avoided, multiple samples can be simultaneously processed, by comparing with a traditional soxhlet extraction method, organic solvent consumption is less, secondary pollution on environment can be avoided, and good extraction effect is reached.
Owner:SHANGHAI ACADEMY OF ENVIRONMENTAL SCIENCES +1
A method for the determination of chlorantraniliprole residues in fruits and vegetables
InactiveCN104459001BAvoid matrix interferenceSimple and fast operationComponent separationEthylenediamineMatrix solution
The invention discloses a method for measuring the residual quantity of chlorantraniliprole in fruit and vegetable. The method comprises performing homogeneous extraction on chlorantraniliprole residue in a sample through acetonitrile or an acetonitrile solution containing 1% of acetic acid; performing dispersed purification on extracted solution through ethylenediamine-N-propyl silicane (PSA) and octadecyl silane bonded phase (C18) matrix; then performing gas chromatograph-negative chemical ionization-mass spectrometry (GC-NCI-MS) detection, establishing a calibration standard curve through blank matrix solution not containing pesticide to be measured, and performing quantitation through the external standard method. The method for measuring the residual quantity of the chlorantraniliprole in fruit and vegetable achieves an average recovery rate of 90.7-101.9%, an average relative standard deviation (RSD) of 5.4-9.6% and a detection limit lower than 0.77 mu g / kg, has the advantages of being convenient and rapid to operate, high in sensitivity and repeatability and accurate in quantitation and quantification, can meet the technical requirements of the corresponding product safety inspection of nations such as the U.S., Japan, the European Union and Canada, and provides powerful technical support for food safety of people and healthy development of export trade in China.
Owner:云南商测质量检验技术服务有限公司
GC-NCI-MS (gas chromatography-negative chemical ionization-mass spectrometry) testing method of residual quantity of cyantraniliprole
ActiveCN104502508AAvoid matrix interferenceSimple and fast operationComponent separationMatrix solutionRelative standard deviation
The invention discloses a GC-NCI-MS (gas chromatography-negative chemical ionization-mass spectrometry) testing method of residual quantity of cyantraniliprole. The method is mainly used for testing the content of cyantraniliprole remained in complex matrix food agricultural products such as cereal grains and animal-origin food. The method comprises the following steps: homogenously extracting cyantraniliprole remained in samples by using acetonitrile or acetonitrile solutions containing 1 percent of acetic acid; purifying and condensing by using a C18 / PSA solid-phase extraction column; detecting by GC-NCI-MS; building a corrected standard curve by using vehicle solutions which do not contain pesticides to be detected; and quantifying by using an external standard method. The method has the average recycling rate of 93.4-97.7 percent, the average relative standard deviation (RSD) of 4.0-7.3 percent and the detection limit of lower than 2.89 microgram / kg, has the advantages of convenience and quickness in operation, good impurity removal effect, high sensitivity, high property, high repeatability and accurate quantitativeness and qualitativeness, and can meet the technical requirement of uniform limit, namely 0.01 mg / kg maximum residue limit of corresponding food security detection, in America, Canada, European Union, Japan and the like, so that powerful technical support is provided for guaranteeing food security of people and healthy development of export trade in China.
Owner:INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
Determining method of Pyrifluquinazon residual quantity
ActiveCN104597189AAvoid matrix interferenceSimple and fast operationComponent separationSilanesRelative standard deviation
The invention relates to a determining method of Pyrifluquinazon residual quantity. The method comprises the following steps: homogeneously extracting residual Pyrifluquinazon in a sample by using acetonitrile or an acetonitrile solution containing 1% acetic acid; after dispersed purification of an extracting liquid by using an ethidene diamine-N-propyl silane (PSA) and octadecyl silane bonded phase (C18) matrix, detecting by gas chromatography-negative chemical ionization-chromatography (GC-NCI-MS); and establishing a corrected standard curve by using a blank substrate solution without to-be-detected pesticides, and quantifying by an external standard method. According to the method provided by the invention, the average recovery rate is 88.7-96.1%, the average relative standard deviation (RSD) is 4.7-6.9% and the detection limit is lower than 0.81 microg / kg. The determining method has the advantages of being simple and convenient to operate, quick, high in sensitivity, good in repeatability and accurate to qualify and quantify and can satisfy the technical requirement on safety detection of corresponding products in countries such as Korea, Japan and European Union, and thus a powerful technical support for guaranteeing the food safety of people in China and healthy development of foreign export trade is provided.
Owner:INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
Detecting method for residual quantity of flubendiamide in fruits and vegetables
ActiveCN104502482AAvoid matrix interferenceSimple and fast operationComponent separationRelative standard deviationFlubendiamide
The invention discloses a detecting method for the residual quantity of flubendiamide in fruits and vegetables. The detecting method comprises the steps of homogenizing by using acetonitrile or an acetonitrile liquid containing 1% acetic acid to extract residual flubendiamide in a sample; dispersing by using a primary secondary amine (PSA) and octadecylsilane bonded-phase (C18) matrix to purify an extracting liquid; then, carrying out gas chromatography-negative chemical ionization-mass spectrum (GC-NCI-MS) detection; establishing a corrected standard curve by using a blank matrix liquid without a pesticide to be detected; and quantifying by using an external standard method. By using the detecting method, the average recovery rate is 93.2-103.1%, the average relative standard deviation (RSD) is 4.6-7.4%, and the detection limit is lower than 1.15mu g / kg; and the detecting method is simple and convenient to operate, rapid, high in sensitivity, good in repeatability and accurate in qualitation and quantitation. According to the detecting method, the technical requirements of America, Japan, European union and other countries on security detection of corresponding products can be met, and the powerful technical support can be provided for ensuring Chinese food safety and the health development of foreign export trade.
Owner:云南通标检测有限公司
GC-NCI-MS (Gas Chromatography-Negative Chemical Ionization-Mass Spectrum) detecting method for residual quantity of cyantraniliprole in fruits and vegetables
ActiveCN104502484AAvoid matrix interferenceSimple and fast operationComponent separationRelative standard deviationHealth development
The invention discloses a GC-NCI-MS (Gas Chromatography-Negative Chemical Ionization-Mass Spectrum) detecting method for the residual quantity of cyantraniliprole in fruits and vegetables. The GC-NCI-MS detecting method comprises the steps of homogenizing by using acetonitrile or an acetonitrile liquid containing 1% acetic acid to extract residual cyantraniliprole in a sample; dispersing by using a primary secondary amine (PSA) and octadecylsilane bonded-phase (C18) matrix to purify an extracting liquid; then, carrying out GC-NCI-MS detection; establishing a corrected standard curve by using a blank matrix liquid without a pesticide to be detected; and quantifying by using an external standard method. By using the GC-NCI-MS detecting method, the average recovery rate is 89.2-96.7%, the average relative standard deviation (RSD) is 3.5-8.8%, and the detection limit is lower than 0.53mu g / kg; and the GC-NCI-MS detecting method is simple and convenient to operate, rapid, high in sensitivity, good in repeatability and accurate in qualitation and quantitation. According to the GC-NCI-MS detecting method, the technical requirements of America, Canada, European union, Japan and other countries on security detection of corresponding products can be met, and the powerful technical support can be provided for ensuring Chinese food safety and the health development of foreign export trade.
Owner:崔淑华
GC-NCI-MS (gas chromatography-negative chemical ionization-mass spectrometry) determination method of residual amount of fluoride ether bacterium amide
ActiveCN104655763AAvoid matrix interferenceSimple and fast operationComponent separationMatrix solutionRelative standard deviation
The invention discloses a GC-NCI-MS (gas chromatography-negative chemical ionization-mass spectrometry) determination method of residual amount of fluoride ether bacterium amide. The method is mainly used for determining the residual amount of fluoride ether bacterium amide in cereal grains, animal-derived foods and other complex matrix food agricultural products. The method comprises the following steps: homogenizing and extracting residual fluoride ether bacterium amide in a sample with acetonitrile or an acetonitrile solution containing 1% of acetic acid, performing purification and concentration by a C18 / PSA solid-phase extraction column, performing GC-NCI-MS detection, establishing a standard curve for correction by adopting a blank matrix solution without a pesticide to be detected, and quantifying by an external standard method. According to the method, the average recovery rate is 85.0%-91.1%, the average relative standard deviation (RSD) is 4.1%-6.6%, the detection limit is lower than 0.35mu g / kg, and the method has the advantages of simplicity and convenience in operation, high speed, good impurity removal effect, high sensitivity, strong characteristic feature, good repeatability and accurate qualitative and quantitative properties. According to the method, the technical requirement of 'being standard without exceptions' of the residual limit of 0.01mg / kg can be met, and a powerful technical support is provided for ensuring food safety of people in China and health development of export trades.
Owner:广东唯诺冠动漫食品股份有限公司
Method for determining residual amount of metrafenone
ActiveCN104655781AAvoid matrix interferenceSimple and fast operationComponent separationMatrix solutionRelative standard deviation
The invention discloses a method for determining residual amount of metrafenone. The method is mainly used for determining the residual amount of metrafenone in cereal grains, animal-derived foods and other complex matrix food agricultural products. The method comprises the following steps: homogenizing and extracting residual metrafenone in a sample with acetonitrile or an acetonitrile solution containing 1% of acetic acid, performing purification and concentration by a C18 / PSA solid-phase extraction column, performing gas chromatography-negative chemical ionization-mass spectrometry (GC-NCI-MS) detection, establishing a standard curve for correction by adopting a blank matrix solution without a pesticide to be detected, and quantifying by an external standard method. According to the method, the average recovery rate is 83.9%-90.1%, the average relative standard deviation (RSD) is 4.0%-5.8%, the detection limit is lower than 0.67mu g / kg, and the method has the advantages of simplicity and convenience in operation, high speed, good impurity removal effect, high sensitivity, strong characteristic feature, good repeatability and accurate qualitative and quantitative properties. According to the method, the technical requirements on safety detection of corresponding products in European Union, United States, South Korea, Japan and other countries can be met, and a powerful technical support is provided for ensuring food safety of people in China and health development of export trades.
Owner:SHENZHEN SINO ASSESSMENT GRP
Detection method for content of brominated flame retardants (BFRs) in food
ActiveCN109061025AMeet detectionOvercome the problem of low recovery rateComponent separationGc nci msCentrifugation
The invention relates to a detection method for content of brominated flame retardants (BFRs) in food. The method comprises the following steps of carrying out microwave-assisted extraction on the food, carrying out centrifugation, collecting supernate, and concentrating the supernate to obtain extract solution; passing a composite column by the extract solution, carrying out elution and collecting eluent; employing a capillary column of which column length is 8-15m, inner diameter is 0.1-0.25mm and liquid film thickness 0.10-0.25mum, detecting the eluent through combination of a GC-NCI-MS selected ion mode (SIM), and carrying out quantitative calculation to obtain the content of the brominated flame retardants through adoption of an external standard method. Compared with a conventional method, the method has the advantages that the method is characterized by simplicity, speediness, accuracy and efficiency, and the lowest detection limit and a recovery rate of a sample and repeated test results satisfy detection for residual quantity of various BFRs in the food such as eggs.
Owner:SUZHOU UNIV OF SCI & TECH
Method for determining residual amount of fluoride ether bacterium amide in vegetables and fruits
ActiveCN104655782AAvoid matrix interferenceSimple and fast operationComponent separationEthylenediamineMatrix solution
The invention discloses a method for determining residual amount of fluoride ether bacterium amide in vegetables and fruits. The method comprises the following steps: homogenizing and extracting residual fluoride ether bacterium amide in a sample with acetonitrile or an acetonitrile solution containing 1% of acetic acid, performing dispersion and purification on an extraction solution with a matrix of ethylenediamine-N-propylsilane (PSA) and octadecylsilane bonded phase (C18), then performing gas chromatography-negative chemical ionization-mass spectrometry (GC-NCI-MS) detection, establishing a standard curve for correction by adopting a blank matrix solution without a pesticide to be detected, and quantifying by an external standard method. According to the method, the average recovery rate is 93.0%-97.1%, the average relative standard deviation (RSD) is 4.1%-6.2%, the detection limit is lower than 2.13mu g / kg, and the method has the advantages of simplicity and convenience in operation, high speed, high sensitivity, good repeatability and accurate qualitative and quantitative properties. According to the method, the technical requirement of 'being standard without exceptions' of the residual limit of 0.01mg / kg can be met, and a powerful technical support is provided for ensuring food safety of people in China and health development of export trades.
Owner:广东南派食品有限公司
Method for measuring residual quantity of chlorantraniliprole in fruit and vegetable
InactiveCN104459001AAvoid matrix interferenceSimple and fast operationComponent separationEthylenediamineMatrix solution
The invention discloses a method for measuring the residual quantity of chlorantraniliprole in fruit and vegetable. The method comprises performing homogeneous extraction on chlorantraniliprole residue in a sample through acetonitrile or an acetonitrile solution containing 1% of acetic acid; performing dispersed purification on extracted solution through ethylenediamine-N-propyl silicane (PSA) and octadecyl silane bonded phase (C18) matrix; then performing gas chromatograph-negative chemical ionization-mass spectrometry (GC-NCI-MS) detection, establishing a calibration standard curve through blank matrix solution not containing pesticide to be measured, and performing quantitation through the external standard method. The method for measuring the residual quantity of the chlorantraniliprole in fruit and vegetable achieves an average recovery rate of 90.7-101.9%, an average relative standard deviation (RSD) of 5.4-9.6% and a detection limit lower than 0.77 mu g / kg, has the advantages of being convenient and rapid to operate, high in sensitivity and repeatability and accurate in quantitation and quantification, can meet the technical requirements of the corresponding product safety inspection of nations such as the U.S., Japan, the European Union and Canada, and provides powerful technical support for food safety of people and healthy development of export trade in China.
Owner:云南商测质量检验技术服务有限公司
GC-NCI-MS determination method for cyenopyrafen residual quantity
ActiveCN104535686AAvoid matrix interferenceSimple and fast operationComponent separationCyenopyrafenMatrix solution
The invention discloses a GC-NCI-MS determination method for the cyenopyrafen residual quantity. The method is mainly used for determining the content of cyenopyrafen residues in complex matrix food-grade agricultural products such as grains and animal-origin foods. Acetonitrile or acetonitrile solution containing 1% of acetonitrile is used for extracting the cyenopyrafen residues in a sample in a homogeneous mode, a C18 / PSA solid-phase extraction column performs purification and concentration, GC-NCI-MS detection is performed, a corrected standard curve is established by the adoption of blank matrix solution not containing pesticides to be determined, and an external standard method is adopted for quantification. According to the method, the average recovery rate is 85.8-91.4%, the average RSD is 4.0-7.0%, the detection limit is lower than 0.44 microgram / kg, and the method has the advantages of being easy and convenient to implement, rapid, good in impurity removal effect, high in sensitivity and characteristic feature, good in repeatability and accurate in quality determination and quantification. The method can meet the requirement of the residue limited quantity of 0.01 mg / kg for corresponding food safety inspection in Japan, EU, Korea and other nations and namely the technical requirement of the uniform standard and will provide forceful technical supports for guaranteeing food safety of Chinese and health development of export trades.
Owner:INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
Method for testing MCCP in plastic or leather product
InactiveCN109142555AEfficient separationExtended service lifeComponent separationGc nci msDissolution
The invention discloses a method for testing MCCP in a plastic or leather product, which comprises the following steps: sampling; pretreating and detecting content of MCCP in a target object after pretreating; wherein the pretreating comprises the following steps of: mixing a sample with an extracting agent and carrying out ultrasonic treatment for a first appointed time period at a first appointed temperature; adding a purifying agent and carrying out ultrasonic treatment for the first appointed time period at the first appointed temperature; taking out an appointed volume of extract liquid for drying and adding a appointed volume of normal hexane for re-dissolution; adding an appointed volume of concentrated sulfuric acid and carrying out vortex for a second appointed time period, and standing a vortex-treated sample solution for a third appointed time. By using the method, each ion pair of MCCP can be effectively separated, the detection accuracy can be improved, by using a GC-NCI-MS analyzer, the use frequency of a chromatographic column is reduced, the service life of the chromatographic column is prolonged, and the instrument response value is proper and meets the general requirement of instrument detection, an average adding standard recovery rate is high, a range of 85-110% can be achieved.
Owner:深圳天祥质量技术服务有限公司
Method for rapidly determining residual fenpyrazamine in animal-derived foods
InactiveCN105717219AAvoid matrix interferenceSimple and fast operationComponent separationLipid formationMatrix solution
The invention discloses a rapid determination method for fenpyrazolone residues in animal-derived foods. The method is mainly used for determining the residual fenpyrazolone content in animal-derived foods with high fat content. Use acetonitrile to homogeneously extract the residual fenpyrazolone in the sample, and the extract solution is dispersed and purified by Enhanced Matrix Removal (EMR) matrix, extracted and concentrated by stripping tube, and then gas chromatography-negative chemical ion source- For mass spectrometry (GC‑NCI‑MS) detection, a blank matrix solution without the pesticide to be tested was used to establish a calibrated standard working curve, and the external standard method was used for quantification. The average recovery rate of this method is 90.4%-93.6%, the average relative standard deviation (RSD) is 5.8%-6.8%, and the detection limit is lower than 3.90 μg / kg. Strong characteristic, good repeatability, accurate qualitative and quantitative advantages. It can meet the technical requirements of the United States, the European Union, Japan and other countries for corresponding product safety testing, and provide strong technical support for ensuring the food safety of our people and the healthy development of foreign export trade.
Owner:郭庆龙
GC-NCI-MS (gas chromatography-negative chemical ionization-mass spectrometry) determination method of residual amount of tetrachlorantraniliprole
ActiveCN104535704AAvoid matrix interferenceSimple and fast operationComponent separationMatrix solutionRelative standard deviation
The invention discloses a GC-NCI-MS (gas chromatography-negative chemical ionization-mass spectrometry) determination method of residual amount of tetrachlorantraniliprole. The method is mainly used for determining the residual amount of tetrachlorantraniliprole in cereal grains, animal-derived foods and other complex matrix food agricultural products. The method comprises the following steps: homogenizing and extracting residual tetrachlorantraniliprole in a sample with acetonitrile or an acetonitrile solution containing 1% of acetic acid, performing purification and concentration by a C18 / PSA solid-phase extraction column, performing GC-NCI-MS detection, adopting a blank matrix solution without a pesticide to be detected to establish a standard curve for correction, and quantifying by an external standard method. According to the method, the average recovery rate is 83.3%-90.3%, the average relative standard deviation (RSD) is 3.5%-6.9%, and the detection limit is lower than 1.43mu g / kg; and the method has the advantages of simplicity in operation, high speed, good impurity removal effect, high sensitivity, strong characteristic feature, good repeatability and accurate quantitative and qualitative properties. According to the method, the technical requirement of 'being standard without exceptions' of the residual limit of 0.01mg / kg can be met, and the powerful technical support is provided for ensuring food safety of people in China and health development of export trades.
Owner:INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
GC-NCI-MS (Gas Chromatography-Negative Chemical Ionization-Mass Spectrum) detecting method for residual quantity of cyenopyrafen in fruits and vegetables
InactiveCN104502510AAvoid matrix interferenceSimple and fast operationComponent separationCyenopyrafenMatrix solution
The invention discloses a GC-NCI-MS (Gas Chromatography-Negative Chemical Ionization-Mass Spectrum) detecting method for the residual quantity of cyenopyrafen in fruits and vegetables. The GC-NCI-MS detecting method comprises the steps of homogenizing by using acetonitrile or an acetonitrile liquid containing 1% acetic acid to extract residual cyenopyrafen in a sample; dispersing by using a primary secondary amine (PSA) and octadecylsilane bonded-phase (C18) matrix to purify an extracting liquid; then, carrying out GC-NCI-MS detection; establishing a corrected standard curve by using a blank matrix liquid without a pesticide to be detected; and quantifying by using an external standard method. By using the GC-NCI-MS detecting method, the average recovery rate is 86.3-94.3%, the average relative standard deviation (RSD) is 4.6-8.6%, and the detection limit is lower than 1.12mu g / kg; and the GC-NCI-MS detecting method is simple and convenient to operate, rapid, high in sensitivity, good in repeatability and accurate in qualitation and quantitation. According to the GC-NCI-MS detecting method, the technical requirements of Korea, Japan, European union and other countries on security detection of corresponding products can be met, and the powerful technical support can be provided for ensuring Chinese food safety and the health development of foreign export trade.
Owner:INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
GC-NIC-MS measurement method for penflufen residual amount
InactiveCN105717213AAvoid matrix interferenceSimple and fast operationComponent separationRelative standard deviationSolid phase extraction
The invention discloses a GC-NCI-MS method for determining the residual amount of flufenapyroxamide, which is mainly used for measuring the residual flufenapyroxystrobale content in complex matrix food and agricultural products such as grains and animal-derived foods. Use acetonitrile or an acetonitrile solution containing 1% acetic acid to homogeneously extract the residual flufenapyramide in the sample, C 18 After purification and concentration of the / PSA solid phase extraction column, gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-MS) detection, a calibration standard working curve is established using a blank matrix solution that does not contain the pesticide to be tested, and the external standard method is used for quantification. The average recovery rate of this method is 88.9%-104.7%, the average relative standard deviation (RSD) is 4.2%-7.5%, and the detection limit is lower than 1.09 μg / kg. Strong characteristics, good repeatability, and accurate qualitative and quantitative advantages. It can meet the technical requirements of the United States, the European Union, Japan and other countries for corresponding product safety testing, and provide strong technical support for ensuring the food safety of our people and the healthy development of foreign export trade.
Owner:崔淑华
Quick measurement method for fluxapyroxad residue in animal derived foods
InactiveCN105699520AAvoid matrix interferenceSimple and fast operationComponent separationGc nci msMatrix solution
Owner:崔淑华
A method for determination of cyantraniliprole residues in fruits and vegetables by gc-nci-ms
ActiveCN104502484BAvoid matrix interferenceSimple and fast operationComponent separationRelative standard deviationChemistry
The invention discloses a GC-NCI-MS (Gas Chromatography-Negative Chemical Ionization-Mass Spectrum) detecting method for the residual quantity of cyantraniliprole in fruits and vegetables. The GC-NCI-MS detecting method comprises the steps of homogenizing by using acetonitrile or an acetonitrile liquid containing 1% acetic acid to extract residual cyantraniliprole in a sample; dispersing by using a primary secondary amine (PSA) and octadecylsilane bonded-phase (C18) matrix to purify an extracting liquid; then, carrying out GC-NCI-MS detection; establishing a corrected standard curve by using a blank matrix liquid without a pesticide to be detected; and quantifying by using an external standard method. By using the GC-NCI-MS detecting method, the average recovery rate is 89.2-96.7%, the average relative standard deviation (RSD) is 3.5-8.8%, and the detection limit is lower than 0.53mu g / kg; and the GC-NCI-MS detecting method is simple and convenient to operate, rapid, high in sensitivity, good in repeatability and accurate in qualitation and quantitation. According to the GC-NCI-MS detecting method, the technical requirements of America, Canada, European union, Japan and other countries on security detection of corresponding products can be met, and the powerful technical support can be provided for ensuring Chinese food safety and the health development of foreign export trade.
Owner:崔淑华
Method for measuring dibromochloropropane residues in fruits and vegetables by GC-NCI-MS
The invention discloses a method for measuring dibromochloropropane residues in fruits and vegetables by GC-NCI-MS. The method comprises the following steps: extraction, purification, preparation of a standard working solution and measurement by gas chromatography-negative chemical ionization-mass spectrometry, and combination of a dispersion solid phase extraction pretreatment technology and a GC-NCI-MS detection technology. The method is quick, simple and convenient; by virtue of utilizing acetic acid or acetonitrile as a solvent, the toxicity is low; the detection limit is as low as 0.75ug / kg, so the sensitivity is high; the recycling rate is 97.40-103.69 percent, so the selectivity is high; the RSD value is 3.02-5.74 percent, so the repetitiveness is high; interference of a matrix is effectively removed, and the method is suitable for detecting dibromochloropropane in various vegetables and fruits and products thereof; meanwhile, methylbenzene is added in the purification step of the dispersion solid phase extraction pretreatment technology, so that adsorption of purification powder PSA to a target is effectively reduced; in the same matrix, the recycling rate of the method is increased from 69.25-75.37 percent without methylbenzene to 97.96-10.3.69 percent.
Owner:广东中检达元检测技术有限公司
Measurement method for fluxapyroxad residue in vegetables and fruits
InactiveCN105699518AAvoid matrix interferenceSimple and fast operationComponent separationEthylenediamineMatrix solution
The invention discloses a method for determining the residual amount of flufenapyroxamide in vegetables and fruits. Acetonitrile or an acetonitrile solution containing 1% acetic acid is used to homogeneously extract the residual flufenapyroxamide in the sample, and the extract is treated with ethylenediamine-N - Propylsilane (PSA) and Octadecylsilane bonded phase (C 18 ) after dispersion and purification of the matrix, gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-MS) detection, a calibration standard working curve was established using a blank matrix solution without the pesticide to be tested, and the external standard method was used for quantification. The average recovery rate of this method is 87.9%-108.1%, the average relative standard deviation (RSD) is 4.7%-8.5%, and the detection limit is lower than 1.59μg / kg. The advantages of quantitative accuracy. It can meet the technical requirements of the United States, the European Union, Japan and other countries for corresponding product safety testing, and provide strong technical support for ensuring the food safety of our people and the healthy development of foreign export trade.
Owner:崔淑华
A kind of assay method of metrafenone residue
ActiveCN104655781BAvoid matrix interferenceSimple and fast operationComponent separationMatrix solutionRelative standard deviation
The invention discloses a method for determining residual amount of metrafenone. The method is mainly used for determining the residual amount of metrafenone in cereal grains, animal-derived foods and other complex matrix food agricultural products. The method comprises the following steps: homogenizing and extracting residual metrafenone in a sample with acetonitrile or an acetonitrile solution containing 1% of acetic acid, performing purification and concentration by a C18 / PSA solid-phase extraction column, performing gas chromatography-negative chemical ionization-mass spectrometry (GC-NCI-MS) detection, establishing a standard curve for correction by adopting a blank matrix solution without a pesticide to be detected, and quantifying by an external standard method. According to the method, the average recovery rate is 83.9%-90.1%, the average relative standard deviation (RSD) is 4.0%-5.8%, the detection limit is lower than 0.67mu g / kg, and the method has the advantages of simplicity and convenience in operation, high speed, good impurity removal effect, high sensitivity, strong characteristic feature, good repeatability and accurate qualitative and quantitative properties. According to the method, the technical requirements on safety detection of corresponding products in European Union, United States, South Korea, Japan and other countries can be met, and a powerful technical support is provided for ensuring food safety of people in China and health development of export trades.
Owner:SHENZHEN SINO ASSESSMENT GRP
A GC‑NCI‑MS method for the detection of dibromochloropropane residues in complex matrices
ActiveCN105223285BEasy to detectEliminate distractionsComponent separationMaterial analysis by electric/magnetic meansGas phaseRelative standard deviation
The invention discloses a GC-NCI-MS method for detection of dibromochloropropane residual quantity in complex matrix. The method is characterized by including the steps of extraction, purification, preparation of a standard working solution and gas chromatography-negative chemical ionization-mass spectrometry (GC-NCI-MS) determination. The solid phase extraction technology and the gas phase chromatography-negative chemical ionization-mass spectrometry (GC-NCI-MS) are combined to realize the qualitative identification and quantitative detection of dibromochloropropane in animal source foods. The method is quick and easy, uses ethyl acetate and acetonitrile as solvents, and has less toxicity. The method has detection limit as low as 0.98ug / kg, high sensitivity, recovery rate of 88.82-94.17%, strong selectivity, relative standard deviation of 2.48-3.77%, and good reproducibility, effectively removes the interference of the matrix, and is applicable to detection of dibromochloropropane in various in animal derived food.
Owner:佛山市金城速冻食品有限公司
A kind of gc-nci-ms assay method of fluoxetin residue
ActiveCN104655763BAvoid matrix interferenceSimple and fast operationComponent separationMatrix solutionRelative standard deviation
The invention discloses a GC-NCI-MS (gas chromatography-negative chemical ionization-mass spectrometry) determination method of residual amount of fluoride ether bacterium amide. The method is mainly used for determining the residual amount of fluoride ether bacterium amide in cereal grains, animal-derived foods and other complex matrix food agricultural products. The method comprises the following steps: homogenizing and extracting residual fluoride ether bacterium amide in a sample with acetonitrile or an acetonitrile solution containing 1% of acetic acid, performing purification and concentration by a C18 / PSA solid-phase extraction column, performing GC-NCI-MS detection, establishing a standard curve for correction by adopting a blank matrix solution without a pesticide to be detected, and quantifying by an external standard method. According to the method, the average recovery rate is 85.0%-91.1%, the average relative standard deviation (RSD) is 4.1%-6.6%, the detection limit is lower than 0.35mu g / kg, and the method has the advantages of simplicity and convenience in operation, high speed, good impurity removal effect, high sensitivity, strong characteristic feature, good repeatability and accurate qualitative and quantitative properties. According to the method, the technical requirement of 'being standard without exceptions' of the residual limit of 0.01mg / kg can be met, and a powerful technical support is provided for ensuring food safety of people in China and health development of export trades.
Owner:广东唯诺冠动漫食品股份有限公司
A kind of gc-nci-ms assay method of tetrachlorantraniliprole residue
ActiveCN104535704BAvoid matrix interferenceSimple and fast operationComponent separationGc nci msMatrix solution
The invention discloses a GC-NCI-MS (gas chromatography-negative chemical ionization-mass spectrometry) determination method of residual amount of tetrachlorantraniliprole. The method is mainly used for determining the residual amount of tetrachlorantraniliprole in cereal grains, animal-derived foods and other complex matrix food agricultural products. The method comprises the following steps: homogenizing and extracting residual tetrachlorantraniliprole in a sample with acetonitrile or an acetonitrile solution containing 1% of acetic acid, performing purification and concentration by a C18 / PSA solid-phase extraction column, performing GC-NCI-MS detection, adopting a blank matrix solution without a pesticide to be detected to establish a standard curve for correction, and quantifying by an external standard method. According to the method, the average recovery rate is 83.3%-90.3%, the average relative standard deviation (RSD) is 3.5%-6.9%, and the detection limit is lower than 1.43mu g / kg; and the method has the advantages of simplicity in operation, high speed, good impurity removal effect, high sensitivity, strong characteristic feature, good repeatability and accurate quantitative and qualitative properties. According to the method, the technical requirement of 'being standard without exceptions' of the residual limit of 0.01mg / kg can be met, and the powerful technical support is provided for ensuring food safety of people in China and health development of export trades.
Owner:INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
GC-NCI-MS method for detection of dibromochloropropane residual quantity in complex matrix
ActiveCN105223285AAchieving qualitative confirmationEasy to detectComponent separationMaterial analysis by electric/magnetic meansGas phaseRelative standard deviation
The invention discloses a GC-NCI-MS method for detection of dibromochloropropane residual quantity in complex matrix. The method is characterized by including the steps of extraction, purification, preparation of a standard working solution and gas chromatography-negative chemical ionization-mass spectrometry (GC-NCI-MS) determination. The solid phase extraction technology and the gas phase chromatography-negative chemical ionization-mass spectrometry (GC-NCI-MS) are combined to realize the qualitative identification and quantitative detection of dibromochloropropane in animal source foods. The method is quick and easy, uses ethyl acetate and acetonitrile as solvents, and has less toxicity. The method has detection limit as low as 0.98ug / kg, high sensitivity, recovery rate of 88.82-94.17%, strong selectivity, relative standard deviation of 2.48-3.77%, and good reproducibility, effectively removes the interference of the matrix, and is applicable to detection of dibromochloropropane in various in animal derived food.
Owner:佛山市金城速冻食品有限公司
A kind of pretreatment method of polybrominated diphenyl ether in environmental solid matrix
ActiveCN104713964BHigh recovery rateMeet trace analysis requirementsComponent separationPretreatment methodDecomposition
The invention relates to a pretreatment method of polybrominated diphenyl ethers in an environment solid matrix, which is characterized in that a combined technology of microwave auxiliary extraction and solid phase extraction is used for processing solid matrix PBDEs such as soil and deposits. The method comprises the following steps: 1)drying and crushing a sample; 2)performing microwave auxiliary extraction: weighing a soil deposit sample to be processed, weighing a certain amount of extraction solvent, using a microwave digestion / extraction instrument for microwave auxiliary extraction; 3)performing solid-liquid separation; 4)solid phase purification and purification by a small column: performing rotary evaporation on the extract to about 1ml, through solid phase extraction and purification by the small column; and 5)subsequent processing: performing nitrogen blowing on an eluate to a dry state, metering volume on the solvent, after membrane filtration, and using GC-NCI-MS for analysis. According to the invention, pre-treatment time of the sample is short, decomposition of unstable substances such as PBDEs can be avoided, multiple samples can be simultaneously processed, by comparing with a traditional soxhlet extraction method, organic solvent consumption is less, secondary pollution on environment can be avoided, and good extraction effect is reached.
Owner:SHANGHAI ACADEMY OF ENVIRONMENTAL SCIENCES +1
A kind of gc-nci-ms determination method of fipronil residues
ActiveCN104407091BAvoid matrix interferenceSimple and fast operationComponent separationMatrix solutionFlubendiamide
The invention discloses a GC-NCI-MS method for measuring residual quantity of flubendiamide. The method is mainly used for measuring the content of residual flubendiamide in complex matrix food agricultural products such as cereal grains and animal derived foods. The method comprises the following steps: homogenizing and extracting the residual flubendiamide in the sample by using acetonitrile or an acetonitrile solution containing 1 percent of acetic acid, purifying and concentrating by using a C18 / PSA solid phase extraction column, performing gas chromatography-negative chemical ion source-mass spectrum (GC-NCI-MS) detection, establishing a corrected standard curve by adopting a blank matrix solution without to-be-detected pesticides, and quantifying by virtue of an external standard method. According to the method, the average recovery rate is 84.2-93.2 percent, the average relative standard deviation (RSD) is 4.6-6.9 percent, the detection limit is lower than 1.44mu g / kg, and the method has the advantages of simplicity and convenience in operation, rapidness, good impurity removal effect, high sensitivity, strong characteristic property, high repeatability and qualitative and quantitative accuracy. The residual limit of 0.01mg / kg in the corresponding food safety inspection in America, Japan, European Union and other countries can be met, namely the technical requirement on uniform limit is met, and a powerful technical support is provided for guaranteeing the food safety and sound export abroad trade development of people in China.
Owner:潍坊海润华辰检测技术有限公司
A kind of assay method of pyrifluquinazon residue
ActiveCN104614478BAvoid matrix interferenceSimple and fast operationComponent separationMatrix solutionRelative standard deviation
Owner:INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
A kind of gc-nci-ms assay method of the residual amount of pyraclofen
ActiveCN104535686BAvoid matrix interferenceSimple and fast operationComponent separationCyenopyrafenMatrix solution
The invention discloses a GC-NCI-MS determination method for the cyenopyrafen residual quantity. The method is mainly used for determining the content of cyenopyrafen residues in complex matrix food-grade agricultural products such as grains and animal-origin foods. Acetonitrile or acetonitrile solution containing 1% of acetonitrile is used for extracting the cyenopyrafen residues in a sample in a homogeneous mode, a C18 / PSA solid-phase extraction column performs purification and concentration, GC-NCI-MS detection is performed, a corrected standard curve is established by the adoption of blank matrix solution not containing pesticides to be determined, and an external standard method is adopted for quantification. According to the method, the average recovery rate is 85.8-91.4%, the average RSD is 4.0-7.0%, the detection limit is lower than 0.44 microgram / kg, and the method has the advantages of being easy and convenient to implement, rapid, good in impurity removal effect, high in sensitivity and characteristic feature, good in repeatability and accurate in quality determination and quantification. The method can meet the requirement of the residue limited quantity of 0.01 mg / kg for corresponding food safety inspection in Japan, EU, Korea and other nations and namely the technical requirement of the uniform standard and will provide forceful technical supports for guaranteeing food safety of Chinese and health development of export trades.
Owner:INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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