381results about How to "Reduce matrix effect" patented technology

The invention discloses a method for determining the content of zinc in the zinc concentrate through energy-dispersive X-ray fluorescence spectrometry. The method comprises the following steps: 1, preparing a plurality of zinc-iron working liquids, converting the mass concentrations of Zn in the operating liquids to Zn mass percentage concentrations, detecting the Zn mass percentage concentrations with an energy-dispersive X-ray fluorescence spectrometer as a detector, recording the fluorescence intensity during each time injection of a sample, and making a working curve; and 2, processing the zinc concentrate as a sample to prepare a sample solution, injecting the sample solution under detection conditions for making the working curve, recording the fluorescence intensity displayed on the detector, reading out the Zn mass percentage concentration corresponded to the fluorescence intensity according to the determined working curve, and calculating according to a specific formula to obtain the mass percentage concentration of simple substance zinc in the sample. The method utilizes a solution process to eliminate or basically eliminate the matrix effect, so the zinc content can be accurately determined; and the method has the advantages of simple operation, short detection period, good detection result accuracy and high precision.

The invention discloses a method for simultaneously detecting forty types of amino acids in dried blood spots, blood and urine. The method comprises the following steps of firstly, pretreating a biological sample by a simple liquid and liquid extracting method; performing chromatographic separation and mass spectrometric detection; using the relative retention time and qualitative ions as the qualitative basis for each type of amino acid, and using a standard product to manufacture a standard curve for quantifying. The method has the advantages that the accuracy and validity of the method shall be studied by three levels of quality control products, so as to avoid the distortion of detection results; the forty types of non-derived amino acids in one sample can be simultaneously detected bya HPLC-MS / MS (high performance liquid chromatography-mass spectrograph) technique for the first time; the operation is simple, convenient and rapid, the flux is high, and the cost is low; the level of amino acids in a human body can be effectively monitored in real time; the enough basis is provided for the clinical disease diagnosis; the method is suitable for being clinically popularized and applied.

A method of quantifying a target analyte by mass spectrometry includes obtaining a mass spectrometer signal comprising a first calibrator signal, comprising a second calibrator signal, and potentially comprising a target analyte signal from a single sample comprising a first known quantity of a first calibrator, comprising a second known quantity of a second calibrator, and potentially comprising a target analyte. The first known quantity and the second known quantity are different, and wherein the first calibrator, the second calibrator, and the target analyte are each distinguishable in the single sample by mass spectrometry. The method also includes quantifying the target analyte in the single sample using the first calibrator signal, the second calibrator signal, and the target analyte signal.

The invention provides a method for measuring residual volatile components in a cigarette filter stick. The method is a headspace-gas chromatography / mass spectrum combined method and adopts an internal standard method to quantify, wherein in the headspace sampling process, N,N-dimethylformamide is used as a substrate correction agent. The method adopts a headspace sampling pretreatment mode, not only is convenient and rapid, but also can reduce loss of a sample due to complex pretreatment; the internal standard gas / mass combined method is adopted for measuring, misjudgment caused by false positive which possibly occurs to a complex system compound is avoided, influence of chromatographic conditions on a quantifying result is reduced and both accuracy and precision are relatively high. The method is used for measuring the volatile components in the cigarette filter stick, is simple, convenient, accurate and rapid to operate, and has good selectivity and strong practical value.

The invention relates to an ICP-MS measuring method of trace metal impurities in high purity lead, which adopts a high-purity nitric acid dissolving sample and uses the electrolytic method to remove lead in the high purity nitric acid dissolving sample, and utilizes inductive coupled plasma mass spectrometer and adopts peak jumping mode to scan and test blank, work-curve standard solution and sample elements to be detected so as to obtain the content of the elements to be detected. The ICP-MS measuring method of trace metal impurities in high purity lead is convenient in operation and can effectively eliminate matrix effect caused by excessively high total solid content and avoid pollution during the preparation process of samples, thus greatly reducing memory effect and obviously increasing measuring accuracy. The ICP-MS measuring method of trace metal impurities in high-purity lead is applicable to the analysis and testing of the content of a plurality of trace metal impurities.

The invention discloses a common rapid detection method for various pesticide residues in soybeans. The common rapid detection method is characterized by particularly comprising the following steps: homogenizing and extracting a soybean sample by acetonitrile; carrying out salting-out and centrifuging to obtain a supernatant; purifying by using a solid phase extraction column to obtain a sampling solution; preparing a mixed standard solution and preparing a base material adding standard curve; simultaneously detecting 306 types of pesticide residues in the soybeans by a gas chromatography-tandem mass spectrometer; finally, calculating the concentration. The common rapid detection method has the advantages that the effect of the base material and background interferences are reduced and the anti-interference capability of the method is improved greatly; the analysis sensitivity is improved; the detection linear range is 0-0.2microgram / milliliter; the detection is limited to be 0.01mg / kg; the recycling rate is 60%-120%; the relative standard deviation RSD is less than or equal to 20%; the recycling rate is ideal and the precision degree is good; the common rapid detection method is simple and rapid, is low in background interferences, good in selectivity and high in sensitivity.

The invention discloses a method for detecting various pesticide residues in tobacco by utilizing a multiwalled carbon nanotube. The method is characterized in that an organic solvent is used for extraction; the multiwalled carbon nanotube is used as a reverse solid phase dispersion adsorbent; the tobacco samples are purified through vortex and centrifugation; a high performance liquid chromatography-tandem mass spectrum coupled technology and a gas chromatography-tandem mass spectrum coupled technology are combined to realize the synchronous detection of various pesticide residues in the tobacco. According to the method, the multiwalled carbon nanotube is used as the reverse solid phase dispersion adsorbent, so that the purification effect, the influence on the adsorption of the target analyte due to the frequently-used polar adsorbents is eliminated while the matrix effects are reduced, and a cleaner solution is provided to decrease the maintenance of the instrument in the using process; the multiwalled carbon nanotube is low in preparation cost and less in dosage and has the effect of greatly reducing the experimental cost; the method provided by the invention has the advantages of being correct in measurement, high in sensitivity and good in repeatability, and has the effect of satisfying the requirement for rapidly analyzing and detecting the large batch samples.

The invention provides a kit for detecting anti-psychosis drugs in a serum and plasma by a liquid chromatography tandem mass spectrometry method. The kit comprises drug standards: amsulpiride, aripiprazole, dehydroaripiprazole, chlorpromazine, clozapine, n-desmethylclozapine, risperidone, 9-hydroxyrisperidone, quetiapine, olanzapine, ziprasidone; drug internal standard compounds: amplepiride-d5, aripiprazole-d8, chlorpromazine-d3, clozapine-d8, risperidone-d4, 9-hydroxyrisperidone-d4, quetiapine-d8, olanzapine-d8, ziprasidone-d8; drug extraction compounds: methanol solution 60% (volume ratio),acetonitrile solution 20%, isopropanol solution 10%, purified water 10%; negative plasma; and a diluent: 50% aqueous methanol solution. The kit can be used to simultaneously detect anti-psychosis drugs and active metabolites thereof, the detection time is short and the flux is large.

The invention provides a method for performing off-line multi-dimensional separation and analysis of a heterogeneous biomolecular sample. The method includes separating the heterogeneous biomolecular sample into a plurality of fractions using an, at least partially, capillary isotachophoresis mechanism. The plurality of fractions are then transferred to a liquid chromatography apparatus where they are each separated into a plurality of sub-fractions. The sub-fractions are then analyzed to determine their constituent molecules.

The invention discloses a method for detecting diarrhea shellfish toxin, which comprises the following steps: A) establishing a standard curve of depolymerization of okadaic acid (OA) induced HL-7702 hepatocyte F-actin; B) carrying out the calculation on the concentration of the OA according to the standard curve of the F-actin depolymerization of the HL-7702 hepatocyte, establishing a detection method of the hepatocyte F-actin of the diarrhea shellfish toxin to determine the possible detection limit range; C) selecting one or more of components (STX, DA and YTX) which are possibly coexist with the diarrhea shellfish to act on the HL-7702 hepatocyte, determining the specificity of the method for detecting the OA content by detecting the degree of damaging the polymerizing power of the HL-7702 hepatocyte F-actin by the above components. The detection method of the invention has the advantages: (1) taking cells as experimental subjects to avoid the using of experimental animals and conforming to the rule of 3R; (2) having high sensitivity; (3) having good specificity; (4) having good repeatability; and (5) having simple and convenient sample extraction and low matrix effects.

The invention discloses a method for simultaneously detecting six types of 24 antibiotics in livestock excrements by combination of ultrasonic extraction-solid phase extraction pretreatment and a liquid chromatography-mass spectrometry technology. The method comprises the following steps: (1) adding an internal standard substance for indicating the recycling rate in advance, and performing ultrasonic extraction; (2) performing solid phase extraction to enrich and purify target antibiotics; (3) performing the liquid chromatography-mass spectrometry technology to detect the contents of the 24 antibiotics. According to the method, the residue conditions of the six types of 24 antibiotics in the livestock excrements can be simultaneously detected at one time; the time of the detection processis short, the detection precision is high, the sensitivity, the stability and the selectivity are high, and the detection limit is low; by optimization of an extraction solvent, chelation between theantibiotics and metal ions in the excrements can be effectively reduced, so that the target antibiotics are separated from a sample, and the recycling rate is increased; furthermore, the method is easy and convenient to operate, high in enrichment factor and high in repetitiveness. The internal standard substance for indicating the recycling rate is added before the whole pretreatment process, sothat the loss of target substances in the pretreatment process can be well expressed, and a final result is more real and reliable.

The invention discloses a quick measurement method for coumarin and safrole in essence and flavor. The quick measurement method comprises the steps of performing oscillation extraction on an essence and flavor sample by taking ethyl alcohol aqueous solution as a solvent, filtering an extracting solution through an organic filtering film, and measuring the coumarin and the safrole through ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS). The quick measurement method has the characteristics that difficulties in quantified separation and purification of a complicated mixture system are avoided through quantification by an isotope dilution internal standard method; the ethyl alcohol aqueous solution is used as the sample extraction solvent, so that the extraction efficiency is guaranteed, and the amount of organic impurities, which enter a chromatographic column, in small samples is reduced; furthermore, the chromatographic column is effectively protected; compared with the conventional method, the UPLC-MS / MS is high in analysis speed, high in repetitiveness and high in recycling rate, and is suitable for analysis of a large batch of samples.

The invention provides an analyzing method for simultaneously determining residues of organophosphorus pesticides and pyrethriods pesticides in soil. The analyzing method is characterized by comprising the following steps: carrying out ultrasonic extraction on a soil test sample by using an acetonitrile solution containing 1% of acetic acid by volume percent; purifying by using a suitable amount of PSA and C18 mixed fillers; blowing liquid supernatant by nitrogen and concentrating until the liquid supernatant is nearly dried; respectively dissolving by acetone and n-hexane and enabling the volume to be constant; raising the temperature by using DB-1701 and HP-5 quartz capillary columns and separating; carrying out GC / FPD (Gas Chromatograph / Flame Photometric Detector) detection and GC / micro ECD (Electron Capture Detector) detection; and finally, quantifying by using a base material external standard method. A test confirms that the method has a wide linear range; the technical indexes including detection sensitivity, accuracy and precision meet the requirements of a residue analysis; the pre-treatment operation is simple, convenient and rapid and a reliable manner is provided for analytical researches for simultaneously determining the residues of ths pesticides and the pyrethriods pesticides in the soil.e organophosphoru.

The method comprises: its standard solution uses the healthy human blood serum as base substance; the fructosamine measuring reagent box uses a combination of dual reagents R1 and R2; said R1 comprises NBT reaction component, pH is neutrality; said R2 is alkalinity potassium carbonate buffer solution; the ratio of R1,P2 to the sample under test is 40-50: 8-12: 3.

The invention discloses an analytical method of simultaneously measuring the residues of organophosphorus pesticide and pyrethriods pesticide in fresh leaves. The analytical method is characterized in that performing supersonic extraction on a tea fresh leaf sample by using an acetonitrile solution with the volume fraction of acetic acid being 1%, purifying by a proper amount of a PSA,C18 and GSB mixing padding, performing nitrogen blowing concentration on supernatant liquid to be almost dried, making up to volume by acetone and normal hexane, performing heating separation by DB-1701 and HP-5 quartz capillary columns, detecting GC / FPD and GC / muECD, and finally performing quantitative measuring by adopting a basic external standard method. Tests show that a linearity range is wide through, technical indexes such as detection sensitivity, accuracy and precision all meet requirements of residue analysis, the pretreatment operation is simple, convenient and rapid, and reliable methods are provided for analytical investigation of simultaneously measuring the residues of the organophosphorus pesticide and pyrethriods pesticide.

The invention discloses a candidate serum calcium standard substance. A method for preparing the candidate serum calcium standard substance comprises the following steps of: diluting in-vitro serum or adding calcium into the in-vitro serum to obtain 5 kinds of serum solution with different calcium concentrations; and fixing a value for each of the 5 kinds of serum solution with different calcium concentrations respectively so as to obtain serum calcium standard substances with 5 calcium concentrations. In the candidate serum calcium standard substance, other substance is not added and only the serum is used as a substrate; the candidate serum calcium standard substance has the advantages of high interoperability, high uniformity, high stability under the -80 DEG C storage condition, reliable traceability of the fixed value and relatively small relative synthesis uncertainty of between 0.83 and 1.55 percent; moreover, compared with other conventional serum calcium standard substances, the candidate serum calcium standard substance has the advantages of low cost and simple preparation method.

The invention discloses a quantitative detection method for pyrethriods pesticide in soil. The method is characterized by comprising the following steps: carrying out ultrasonic extraction on a soil sample by using an acetonitrile solution of which the volume fraction is 1%, purifying by using proper mixed filler of PSA and C18; carrying out nitrogen blowing and concentrating on supernate until nearly dry; dissolving and metering volume by using normal hexane; heating up and separating by using HP-5 quartz capillary column program; carrying out GC / muECD detection; finally quantifying by using a matrix external standard method. A test proves that the method is wide in linear range, the technical indicators such as the detection sensitivity, the accuracy and the precision meet the requirements of residue analysis, the quantitative detection method is simple in pre-treatment operation, convenient and fast, and reliable means is provided for analysis and research of pyrethriods pesticide residue in the soil.

The invention discloses a method for simultaneously detecting multiple anti-tumor drugs in a blood sample. A pretreated sample to be detected is detected by adopting ultra-high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS). The pretreatment process comprises the following steps: adding serum into a mixed solution of methanol and acetonitrile, oscillating and centrifuging,taking out the centrifuged supernatant, drying, dissolving the dried powder into a methanol aqueous solution, and filtering to obtain a sample to be detected. The method can be used for simultaneously detecting 13 kinds of anti-tumor drugs such as methotrexate, 5-fluorouracil, apatinib, busulfan, carboplatin, cyclophosphamide, docetaxel, gemcitabine, imatinib, illinotecan, lenalidomide, oxaliplatin, paclitaxel and the like in blood.

The invention discloses an immune-fluorescence test strip component for rapidly detecting C-reactive protein quantitatively, a detection card component produced by the same and a method for preparing the same. The test strip component comprises a test strip and a platinum porphyrin marked specific antibody independently packed. The test strip comprises a bottom lining, a water absorption pad, coating analysis film and a sample pad. The coating analysis film is provided with a detection line and a quality control line, a specific antibody coated by the detection line is a C-reactive protein resistance monoclonal antibody, and a specific antibody coated by the quality control line is a rabbit intravenous gamma globulin (IgG) antibody; the detection card component comprises a test strip, a card box composed of a cover plate and a back plate and a latinum porphyrin marked specific antibody independently packed. The test strip component for detecting C-reactive protein in body fluid has the advantages of being simple in operation, rapid, sensitive, good in specificity and the like, and having good clinical application prospect.

The invention discloses a full-scan and high-throughput rapid screening detection method for illicit drugs in a health food. Data-dependent acquisition (IDA-MS) and data-independent acquisition (SWATH-MS) high-resolution mass spectrometry technologies are combined with Chemspider and an ACS compound structure database, illegally added western medicine ingredients in the health food are rapidly screened and analyzed according to the accurate parent ion and fragment molecular weights of primary mass spectrometry and secondary mass spectrometry and isotope peaks and other high-resolution mass spectrometry data information in the absence of a standard substance, and illicit drug ingredients in the health food are qualitatively identified under an unknown target substance condition in order toovercome the non-target substance detection problem of the health food. The method has the advantages of high-throughput analysis of the target substances, small matrix effect, high accuracy, simplicity in pretreatment, fastness, accuracy, small false negative error and small false positive error.

The invention belongs to the field of drug detection, and particularly relates to a method and a kit for detecting five psychotropic drugs and main metabolites thereof in blood. The five psychotropicdrugs and the main metabolites thereof comprise: olanzapine and demethyl olanzapine, risperidone and 9-hydroxy risperidone, aripiprazole and dehydrogenated aripiprazole, Escitalopram and demethyl citalopram, sertraline and N-demethyl sertraline. Accoridng to the method provided by the invention, a pair of quantitative ion pairs is respectively selected for each detection substance, a relative retention time thereof is used as a qualitative basis, and a standard curve is made by using a standard product for quantification; furthermore, the accuracy and effectiveness of the method are evaluatedfrom quality control of three low, middle and high levels, thereby avoiding distortion of the detection result; and meanwhile, an internal standard working solution is applied to correction, so that matrix effects can be avoided, and accurate quantification is realized. The method provided by the invention has the advantages of simple and rapid operation, high flux and low cost, and can be appliedto the therapeutic drug monitoring of the psychotropic drugs in the clinical work of the psychiatry department.

The invention discloses a pre-treatment method of detection of a liquid sample with laser-induced breakdown spectroscopy. The pre-treatment method includes the steps of paving high-water-absorption resin in a container, adding the liquid sample into the container, and performing vibration to form gel. The invention also provides the detection method of the liquid sample with the laser-induced breakdown spectroscopy. The method greatly increases signal intensity of the liquid sample with laser-induced breakdown spectroscopy during detection, is low in intensities of a background signal and a noise signal, is high in signal-to-background ratio and signal-to-noise ratio, and greatly and effectively increases the sensitivity and accuracy of detection of the liquid sample.

The invention discloses a standard serum cholesterol substance and the application thereof. The standard serum cholesterol substance is prepared by a method with the following steps: (a) pellucid bovine serums are chosen and classified according to initial values that are measured by adopting a cholesterase method; (b) a high-concentration cholesterol concentrated solution is prepared by adopting an ultracentrifugation method, and an initial value is measured by adopting the cholesterase method; (c) a preparation concentration is preset, and a preparation proportion is computed for the preparation according to a required preparation content and the bovine serum classification; (d) an antiseptic agent is added; and (e) the product is filtered and separately packaged, wherein, sodium azide is taken as the antiseptic agent, with the usage ratio of 0.1 percent according to the weight and volume ratio, and the filtering carries out the aseptic filtering by using an asbestos filtering plate of 0.2 micrometer. The result of a series of experiments that are implemented by adopting the standard bovine serum cholesterol substance obtained by the invention indicates that the standard substance has small matrix effect, universality in partial systems, uniformity and good stability.

The invention relates to the technical field of biological detection, and specifically relates to a calibration product and quality control product for the mass spectrometry detection of vitamin D andmetabolite thereof, and a preparation method and applications thereof. The provided calibration product or the quality control product includes a matrix and one or more kinds selected from vitamin Dand metabolite thereof; and the matrix includes polysaccharide substances, protein substances, phospholipid, an electrolyte conditioning agent, a surfactant and a preservative. The matrix effects during sample detection can be effectively reduced by developing a matrix formula of the calibration product and quality control product for the mass spectrometric detection of the vitamin D and metabolite thereof; the calibration product including the provided matrix can realize the high accuracy of mass spectrometry detection systems of the vitamin D and metabolite thereof; and the quality control product including the provided matrix can guarantee the indoor precision of the mass spectrometry detection systems of the vitamin D and metabolite thereof.

The invention relates to a method for determining the content of hydrocarbons and oxygen-containing compounds in Fischer-Tropsch synthetic oil. The method comprises the following steps: separating theFischer-Tropsch synthetic oil through a solid-phase extraction method to obtain a hydrocarbon mixed component and an oxygen-containing compound mixed component; carrying out gas chromatography-massspectrometry analysis, determining a reference component in an obtained spectrogram, calculating a retention index of each peak, determining hydrocarbons or oxygen-containing compounds corresponding to each peak according to the retention indexes and a compound qualitative database, and obtaining the content of each hydrocarbon or oxygen-containing compound according to the peak area. Compared with the prior art, according to the invention, the method has the advantages that rapid separation of hydrocarbons and oxygen-containing compounds in the Fischer-Tropsch synthetic oil is realized through a solid phase extraction method, mutual interference of hydrocarbons and oxygen-containing compounds in the Fischer-Tropsch synthetic oil in retention time is effectively eliminated through GC-MS, and rapid qualitative and quantitative analysis of each component is realized in combination with qualitative advantages of GC-MS and a simple data processing algorithm.

The invention, which belongs to the technical field of tobacco component detection, relates to an analytical method for quantitatively measuring super-multi-target aroma components in tobacco. The method comprises the following steps that: a tobacco sample is immersed in an acidic buffer solution and extraction is performed by an organic solvent; a multi-walled carbon nanotube is used as a reversesolid phase-dispersed adsorbent and vortexing and centrifugation are performed to purify the sample; and then simultaneous detection of 345 kinds of aroma component in tobacco is realized by combining gas chromatography-tandem mass spectrometry. The method has advantages of simple and rapid operation, high flux, low cost, low solvent dosage, good environmental friendly effect, wide range of analytical compounds, high accuracy, high precision, high sensitivity and high repeatability and can satisfy the demand of rapid detection and analysis of aroma component in tobacco.

The invention provides a method for detecting retinol and a precursor thereof. The method comprises the following steps: 1, extracting retinol and / or the precursor thereof from a sample; 2, separating retinol and / or the precursor thereof through HPLC; and 3, carrying out MS / MS quantitative detection, wherein the sample is a dry blood spot card sample, and an extractant adopted in the invention is trichloromethane. A filter paper card is adopted as a carrier to adsorb a tiny amount of blood in order to make the dry blood stop card, so the difficulties of much blood induced by venous blood collection, bad population compliance, death induced by animal model blood drawing, and inconvenient long-distance conveying of samples in previous serum collection and detection process are overcome. The method has the advantages of small matrix effect, good linear relation of analysis in the concentration range of a standard curve, low detection limit, high sensitivity, good accuracy and high precision, is related with the result of detection of retinol in serum through HPLC, allows the contents of the retinol and the precursor thereof in the sample to be simultaneously and synchronously analyzed, and provides a method for comprehensive assessment of the in vivo retinol level.

The invention discloses a preparation method of a solid phase extraction column of molecular imprinted of phenolic environmental estrogens. The method comprises steps of: uniformly mixing 100-500mg of molecular imprinted polymer of phenolic environmental estrogens with 5-20mL of pure organic solvent, and uniformly mixing 100-500mg of traditional solid phase extraction packing with 5-20mL of pure organic solvent; orderly moving the mixtures into a hollow solid phase extraction column; plugging two ends of the solid phase extraction column with sieve plates; adding an acid organic solvent into the solid phase extraction column to wash after the solid phase extraction column being uniformly filled; flushing the filled solid phase extraction column with the pure organic solvent; purging the filled solid phase extraction column with inert gases to remove residual organic solvent; and drying to obtain the product. The preparation method disclosed by the invention is simple, and has particularity matching with the molecular imprinted polymer of phenolic environmental estrogens; and the prepared solid phase extraction column performs high selectivity and high recovery rate to the phenolic environmental estrogens, and is capable of obviously reducing the matrix effects.

The invention provides a kit for determining antianxiety / hypnotic type drugs in serum and plasma through liquid chromatography tandem mass spectrometry. The kit comprises the following constituents: drug standards comprising bromazepam, clonazepam, diazepam, lorazepam, midazolam, nitrazepam, oxazepam and Temazepam; drug internal standard compounds comprising alprazolam-d5, clonazepam-d4, diazepam-d5, lorazepam-d4, midazolam-d4, nitrazepam-d5, oxazepam-d5 and Temazepam-d5; drug extraction compositions comprising, by volume, 60% of methanol solution, 20% of acetonitrile solution, 10% of isopropanol solution and 10% of purified water; negative plasma; and diluent: 50% of carbinol water solution. The kit can be used for simultaneously determining antianxiety / hypnotic type drugs and active metabolites thereof, and has the advantages of short determination time and high flux.