43 results about "Gc nci ms" patented technology

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.

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.

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.

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.

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.

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.

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.

The invention discloses a determination method for Pyrifluquinazon residual quantity. The method is mainly used for determining the content of residual Pyrifluquinazon in complex matrix food and agricultural products such as cereal grains and animal derived foods. Homogeneous extraction of residual Pyrifluquinazon in samples is carried out by using acetonitrile or an acetonitrile solution containing 1% of acetic acid, after purification and concentration with a C18 / PSA solid-phase extraction column, gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-MS) detection is carried out, a corrected standard curve is established by adopting a blank substrate solution which does not contain a pesticide to be tested, and quantization is carried out by an external standard method. According to the method, the average recovery rate is 75.1%-80.2%, the average relative standard deviation (RSD) is 4.8%-8.0%, the detection limit is lower than 2.77 microg / kg, and the determination method has the advantages of easiness, convenience and quickness in operation, good impurity removal effect, high sensitivity, marked characteristics, good repeatability, and accurate qualification and quantization. The determination method can meet the technical requirement of countries such as Japan, European Union and South Korea for 0.01mg / kg residue limit in corresponding food safety testing, namely 'uniform standard', so as to provide powerful technical support for guaranteeing the food safety of Chinese people and the healthy development of export trade.

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.