31 results about "Hplc icp ms" patented technology

The invention relates to a detection method of selenium forms in plants. The method comprises the steps of: 1, previous preparation of detection: determining instruments and reagents for detection; 2, establishing high performance liquid chromatography and inductively coupled plasma mass spectrometry, that is, HPLC-ICP-MS hyphenated techniques; 3, establishing chromatograms of five selenium form standard solutions; 4, pretreatment of plant samples and extraction and detection of selenium forms: cleaning plant materials to be detected with ultrapure water, carrying out freeze drying, smashing and filtering, measuring the water content, sealing, placing and storing at 4 DEG C for standby; or performing ultrasonic extraction at 37 DEG C for 30 minutes by enzyme immediately, taking supernatant after centrifugalization, detecting the selenium forms according to the HPLC-ICP-MS hyphenated techniques, and calculating the content of selenium forms in plants according to peak areas corresponding to the selenium forms in the samples shown in collected maps. According to the method for detecting the selenium forms in plants, forms are separated completely, pretreatment of samples is simple, convenient and rapid, the moving phase is single in component and simple to prepare, the repeatability and the precision are good, and the quantitative result is accurate and reliable.

A method for detecting a divalent cadmium ion in an aquatic product by using an HPLC-ICP-MS (High Performance Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometer) coupling technique belongs to the technical field of detection of aquatic products. The method comprises the following steps: 1), selecting instruments and equipment as well as an HPLC-ICP-MS coupling system; 2), configuring reagents and a standard solution; 3), processing a sample; 4), creating conditions for the experiment instruments; and 5), detecting the sample and calculating the results. According to the method, the cadmium in the aquatic product is extracted by neutral water in an ultrasonic way and the state of the cadmium is not changed, so that the cadmium in a free ion state and the cadmium subjected to complexation with organic matters such as protein both exist in the extract solution. In the adopted mobile phase, oxalate exerts a strong complexation effect on the cadmium ions but does not adsorb and elute stable cadmium complex in the extract solution, so that the cadmium ions and the cadmium complex in the sample can be guaranteed to be better separated. The method for detecting the divalent cadmium ion in the aquatic product by using the HPLC-ICP-MS coupling technique fills a blank in national standard that only the cadmium detection method is provided but no method for detecting the state of cadmium element is provided, therefore, the quality safety of the aquatic product and products of the aquatic product can be accurately and scientifically evaluated, meanwhile, the method is of great significance for formulating a new standard on the limit of harmful elements in the aquatic product.

The invention discloses a method for detecting alkyl mercury in water based on a solid-phase extraction gathering and liquid-phase chromatograph-ICP-MS combined technology. The method comprises the following steps: a, gathering an alkyl mercury mixed standard series in a solid phase extraction manner; b, determining the gathered alkyl mercury mixed standard series by utilizing HPLC-ICP-MS to obtain a linear relation equation between the concentration of the standard series and an area of a chromatographic peak; c, gathering alkyl mercury in an unknown water sample in a solid-phase extraction manner; d, determining the gathered alkyl mercury of the unknown water sample by utilizing PLC-ICP-MS, substituting the obtained peak area into the linear equation, and calculating to obtain the concentration of the alkyl mercury in the water. By adopting the method, the linear detection range of the alkyl mercury is wide, and the detection limit is low. The method has characteristics of simplicity in operation, high accuracy, high sensitivity, high automation degree, environmental friendliness and the like and is suitable for determining alkyl mercury in surface water, water from sewage factories and water in water supply pipe network.

The invention discloses a method for separating and determining chromium elements with different valences in tobacco and tobacco products. The method comprises the following steps of 1, selecting apparatuses and equipment, wherein the separation and determination device is a high performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS) combined device, 2, preparing a reagent and a standard solution, 3, pretreating a sample, 4, determining the sample and calculating and expressing a calculation result. The method utilizes the HPLC-ICP-MS combined technology to realize separation and determination of chromium elements with different valences in tobacco and tobacco products, has good effects of analysis, determination and separation of chromium elements with different valences, a low detecting limit, high sensitivity and good repeatability, can detect chromium elements with different valences in a sub-concentration (microgram / liter) level, and in other word, can detect content of Cr(III) and Cr(VI) in tobacco and tobacco products. The method for separation and determination optimizes a sample pre-treatment process and simplifies separation and determination processes.

The invention discloses a method for synchronously detecting a content of food additives and heavy metals in food in an inverse HPLC-ICP-MS method. The method comprises the following steps: connecting an HPLC device and an ICP-MS device by virtue of a dedicated interface system (5) of Agilent company, detecting the content of the food additives in a processed food sample by virtue of HPLC, and then inputting the food sample flowing by the HPLC into the ICP-MS to perform the heavy metal content detection by virtue of the interface system (5). By adopting the method, the content of the food additives and heavy metals in the food can be rapidly, accurately and synchronously detected, not only can the sampling amount of the sample to be detected and the pretreatment amount of the sample be reduced, but also the operation complexity caused by separate detection and separate sample feeding of different instruments can be reduced, the detection time is greatly shortened, and the working efficiency is improved. The detection time of the two instruments is respectively about 6 hours, and after the two instruments are combined to use, the time is about 4.8 hours, and the time is saved by about 20 percent.

The invention aims at providing a method for identifying wild and artificial cordyceps sinensis. Based on the routine detection of arsenic and arsenic forms in cordyceps sinensis, the content of totalarsenic, inorganic arsenic and organic arsenic in wild and artificial cordyceps sinensis is determined by inductively coupled plasma mass spectrometry (ICP-MS) and anion exchange high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS). The content of inorganic arsenic relative to total arsenic in wild cordyceps sinensis is lower than that in artificial cordyceps sinensis, the percentage of content of inorganic arsenic in content of total arsenic in the wild cordyceps sinensis is lower than 10%, and the content of inorganic arsenic relative to total arsenic in artificial cordyceps sinensis is higher than 30%; in the wild cordyceps sinensis, the content of unknown organic arsenic accounts for 89%-92% of that of total arsenic, and in artificial cordyceps sinensis, the content of unknown organic arsenic accounts for 51%-65% of that of total arsenic. The identification method is simple in decision, saves time and labor, and is low in cost.

The invention discloses an ultrasonic assisted HPLC-ICP-MS detecting and analyzing method for different arsenic form component content in complementary foods for infants. The method comprises the following steps: 1) after the to-be-detected sample of complementary foods for infants is pretreated, extracting by using a methanol aqueous solution and an enzyme solution to obtain a to-be-measured liquid; 2) separating different arsenic form components of the to-be-detected liquid by using high performance liquid chromatography; and 3) measuring different arsenic form components by using the CCT mode of ICP-MS. According to the ultrasonic assisted HPLC-ICP-MS detecting and analyzing method for different arsenic form component content in complementary foods for infants, an arsenic form liquid chromatography-inductively coupled plasma mass spectrometry combined analysis method is established, the extracting method and chromatographic conditions of the arsenic form in various types of complementary foods for infants are optimized. The method is suitable for actual detection of various types of complementary foods for infants and has the advantages of being efficient, fast, accurate and thelike.

The invention provides a method for detecting tributyltin in marine fishes and shellfishes. The method comprises the following steps: taking a to-be-detected sample, adding a standard TBT solution into the to-be-detected sample, and performing ultrasonic extraction with an acetic-acid-methanol solution to obtain a to-be-adsorbed solution; preparing Fe3O4 nanoparticles, modifying the Fe3O4 nanoparticles with APTS, modifying the obtained Fe3O4@APTS particles with MAA, and coating the obtained Fe3O4@MAA particles with an MIP layer to obtain a magnetic molecularly imprinted polymer Fe3O4@MIPs; and adding the to-be-adsorbed solution into Fe3O4@MIPs for adsorption while performing magnetic stirring, performing elution with a formic-acid-methanol solution, and detecting the obtained eluate with HPLC-ICP-MS. The method has characteristics of good interference resistance and high sensitivity and speed. At the same time, according to the method, gathering of tributyltin is improved during a detection process and provides necessary requirements for detection, and adoption of the imprinted polymer is beneficial for specificity detection.

The invention discloses a method for determining the form and valence content of arsenic in biological tissues and organs. Arsenic in it; (2) Determination of total arsenic content in biological organism samples by ICP-MS. The invention also discloses a method for measuring the content of valence arsenic in biological organisms, which is characterized in that the method comprises the steps: (1) the biological organism samples are sequentially pretreated, enzymatically hydrolyzed and filtered, thereby extracting the valence arsenic therein; ( 2) Determination of valence arsenic content in biological organism samples by HPLC-ICP-MS method. The method is simple and feasible, not only can effectively and completely extract the arsenic in the biological body, but also can ensure the stability of the valence arsenic.

The invention discloses a quick determination method of speciation mercury in liquefied natural gases. The quick determination method includes steps of solution preparation, sample pretreatment, HPLC-ICP-MS instrument condition and result determination, result calculation, etc. The quick determination method of speciation mercury in liquefied natural gases is convenient, quick and accurate.

The invention discloses an HPLC-ICP-MS combined method for measuring arsenic form in soil. Phosphoric acid-ascorbic acid is used as an extraction solution for performing sample pretreatment by microwave-assisted extraction, and qualitative and quantitative analysis on ten arsenic forms in the soil is carried out by combining a detection means of liquid chromatography inductive coupling plasma massspectrometry. The method disclosed by the invention is rapid and simple, has relatively high sensitivity and lower detection limit, and is accurate and reliable in determination result and capable ofmeeting the simultaneous measurement of various forms of arsenic in soil.

The invention discloses a method for determining the content of organic selenium in a selenium-rich peanut and a product prepared from the selenium-rich peanut. The method comprises the following steps: 1) mixing a sample to be tested with enzyme to obtain a mixture; 2) sequentially performing ultrasonic-assisted extraction and constant-temperature water bath oscillation on the mixture, centrifugally separating and taking liquid supernatant and residues; performing mixture treatment on the residues to obtain liquid supernatant 1 and residues 1; 3) taking the liquid supernatant and the liquid supernatant 1 and detecting the content of organic selenium by adopting an HPLC-ICP-MS method; 4) summating the content of the organic selenium in the liquid supernatant and the liquid supernatant 1 to obtain the content of organic selenium in the sample to be tested and a selenium-rich wheat standard substance. According to the method disclosed by the invention, the content of the organic selenium in the selenium-rich peanut and the product prepared by the selenium-rich peanut can be more accurately determined.

The invention relates to a method for measuring the concentrations of four arsenic compounds in granulocytes by using an HPLC (High Performance Liquid Chromatography)-ICP (Inductively Coupled Plasma)-MS method and an application, and belongs to the technical field of blood sample detection. In order to solve the problem that the existing method cannot accurately measure the concentrations of fourdifferent arsenic compounds AsIII, AsV, DAV and MMVA in granulocytes, the invention provides a method for measuring the concentrations of four arsenic compounds in granulocytes by using the HPLC-ICP-MS method. The method comprises the steps of determining a detection condition, preparing a standard solution, drawing a standard curve, collecting and processing a granulocyte sample, performing sample detection and data processing. According to the method for measuring the concentrations of four arsenic compounds in granulocytes by using the HPLC-ICP-MS method and the application, each arsenic compound in granulocytes can be effectively extracted and accurately quantified. When the method is applied to the detection of the concentrations of four arsenic compounds in peripheral blood granulocytes of a patient suffering from APL (Acute Promyelocytic Leukemia, the metabolism and distribution characteristics of each arsenic form can be clarified, a technical basis is provided for revealing ofthe action mechanism of arsenic acid and reduction of toxic reactions, and when the method is used for assisting clinics, personalized medicine and targeted therapy are implemented.

The invention discloses methods for determining total amount mercury and valence mercury content in biological tissues and organs. The method comprises the following steps: 1) pretreatment, enzymolysis, filtration and decomposition are carried out on a biological tissues sample in order, and thereby mercury is extracted; and 2) an ICP-MS method is used for determining the total amount mercury content in the biological tissues sample. The invention also discloses a method for valence mercury content in biological mechanism, the method comprises the following steps: 1) pretreatment, enzymolysis, and filtration are carried out on a biological mechanism sample in order, and thereby valence mercury is extracted; and 2) a HPLC-ICP-MS method is used for determining the valence mercury content in the biological mechanism sample. The method is simple and feasible, can effectively and completely extract the mercury in the biological mechanism, and can grantee the stability of the valence mercury.

The invention provides detecting of different arsenic forms in environmental water based on an HPLC-ICP-MS hyphenated technology. Detecting specifically comprises the steps that (1) a mixed standard solution is collocated, specifically, flowing phase L-aminothiopropionic acid serves as a solvent to collocate an arsenic mixed standard solution; (2) standard curves are drawn, specifically, the mixedstandard solution prepared from the step 1 is taken, the arsenic form concentration is detected by using the HPLC-ICP-MS, and according to the arsenic form concentration in the mixed standard solution and corresponding signal intensity, the standard curves of arsenic forms are drawn; (3) pretreatment is conducted on a sample, specifically, a to-be-detected water sample passes through a 0.45 [mu]mfilter membrane before sampling, a KOH solution is added, the sample is placed in a 4 DEG C low temperature condition after sampling, in experiment, the to-be-detected sample is measured out to a centrifuge tube, a flow phase is added to serve as a to-be-detected sample solution, and meanwhile blank test is carried out; and (4) the sample is detected, specifically, the HPLC-ICP-MS is used for measuring and analyzing the arsenic form concentration in the to-be-detected sample solution, the respective concentration value of the arsenic forms in the to-be-detected sample are calculated and analized according to RSD (relative standard deviation) of signal intensity obtained by calculating and the respective standard curves of the arsenic forms.

The invention discloses a morphological analysis method for selenium in selenium-rich protein polysaccharide. The method includes the steps that protease XIV is added into selenium-rich protein polysaccharide, ultrasound-assisted enzymolysis is carried out, and high performance liquid chromatography-inductively coupled plasma-massspectrometry (HPLC-ICP-MS) is adopted to analyze selenium compounds in enzymolysis supernate, wherein the selenium compounds include selenocystine (SeCys2), selenocysteine (SeCys) and sodium selenite (Na2SeO3). The method meets the requirements for environmental friendliness and economy, enzymolysis lasting for 24 h or a longer time is not needed, and the recovery rate is higher than that of a common method.

The invention discloses a determination method for arsenic of four forms in imported liquefied natural gas. The method comprises the steps of solution preparation, sample pretreatment, HPLC-ICP-MS condition and result determination, result calculation and the like. The determination method is convenient, rapid and accurate to implement.

The present invention relates to the field of biological detection technology, relates to a method for quantifying transferrin in human serum by nanogold labeling and liquid chromatography mass spectrometry, and particularly relates to a method for quantitative detection of the transferrin in the human serum through high performance liquid chromatography (HPLC) and inductively coupled plasma mass spectrometry (ICP-MS) based on the nanogold labeling. The method comprises following steps: (1) preparing nano gold particles: (2) using nanogold to label the transferrin in the human serum albumin; and (3) using HPLC-ICP-MS to measure the transferrin in the serum. The method is successfully applied to detection of the transferrin in human serum samples, and has a recovery rate of between 93.0 and 99.7%. Due to efficient separation of the HPLC and ultrasensitive detection of the ICP-MS, the method has potential to simultaneously measure multiple low-abundance markers in biological samples.

The invention relates to a method for detecting inorganic lead ions in marine shellfish by using HPLC-ICP-MS coupling technique, and belongs to the field of food detection. The method for detecting the inorganic lead ions in the marine shellfish by using the HPLC-ICP-MS coupling technique comprises the following steps that (1) an HPLC-ICP-MS coupling system is used as a selected and used instrument and equipment; (2) a reagent and a standard solution are configured; (3) sampling treatment is carried out; (4) instrument conditions used by an experiment are included; and (5) sample detection andresult calculation are carried out. A cation-exchange chromatography can absorb the inorganic lead ions in a sample extracting solution, the inorganic lead ions are eluted through a complexing actionof oxalic acid to lead ions in flow phase, and the inorganic lead ions are analyzed through an inductively coupled plasma source mass spectrometer to obtain retention time of the inorganic lead ionsand pulse strength of a degree of separation of the inorganic lead ions. An equation of linear regression is obtained by instrument computer fitting according to integrals of the strength of a standard series solution and the pulse strength. According to the method for detecting the inorganic lead ions in the marine shellfish by using the HPLC-ICP-MS coupling technique, an inorganic lead element in aquatic products can be accurately detected, quality safety of the aquatic products and products of the aquatic products can be accurately and scientifically evaluated, and meanwhile, an important significance is provided for setting a new standard for limiting harmful elements in the aquatic products.

The invention provides a method for detecting different mercury forms in an environmental water body based on HPLC-ICP-MS coupling. The method comprises the concretely steps of: (1) preparation of a mixed standard solution: preparing a mercury mixed standard solution by taking a mobile phase L-cysteine as a solvent; (2) drawing of a standard curve: taking the mixed standard solution prepared in the step (1), determining the concentration of the mercury form by using HPLC-ICP-MS, and drawing a standard curve of the mercury form according to the concentration of the mercury form in the mixed standard solution and the corresponding signal intensity; (3) sample pretreatment: prior to sampling, allowing a water sample to be tested to be filtered by a 0.45 [mu]m filter membrane, adding a KOH solution, storing the water sample at a low temperature of 4 DEG C after sampling, during an experiment, measuring the sample to be tested, putting the sample to be tested into a centrifuge tube, adding a mobile phase as a solution of the sample to be tested, and performing a blank test; and (4) sample detection: determining and analyzing the concentration of the mercury form in the solution of the sample to be tested by using HPLC-ICP-MS, and calculating and analyzing the concentration value of the mercury form in the sample to be tested according to the relative standard deviation RSD of the calculated signal intensity and the respective standard curve of the mercury form.

The invention discloses a separation measurement method for mercury elements with different valences in bolete. The method includes the following steps that 1, instruments and equipment are selected,wherein a high-performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS) serves as the separation measurement equipment; 2, a reagent and a standard solution are prepared; 3, sample pretreatment is conducted; 4, sample measurement and result calculation and expression are conducted. The separation measurement method optimizes the preprocessing steps of samples, the separation measurement process is simplified, the detection linear range is wide, the detection limit is low, and the method has the advantages of being easy and rapid to operate, high in accuracy,high in sensitivity, and high in automation level.

The invention aims at providing a method for identifying wild and artificial cordyceps sinensis. Based on the routine detection of arsenic and arsenic forms in cordyceps sinensis, the content of totalarsenic, inorganic arsenic and organic arsenic in wild and artificial cordyceps sinensis is determined by inductively coupled plasma mass spectrometry (ICP-MS) and anion exchange high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS). The content of inorganic arsenic relative to total arsenic in wild cordyceps sinensis is lower than that in artificial cordyceps sinensis, the percentage of content of inorganic arsenic in content of total arsenic in the wild cordyceps sinensis is lower than 10%, and the content of inorganic arsenic relative to total arsenic in artificial cordyceps sinensis is higher than 30%; in the wild cordyceps sinensis, the content of unknown organic arsenic accounts for 89%-92% of that of total arsenic, and in artificial cordyceps sinensis, the content of unknown organic arsenic accounts for 51%-65% of that of total arsenic. The identification method is simple in decision, saves time and labor, and is low in cost.

The invention discloses a determination method for arsenic of four forms in imported liquefied natural gas. The method comprises the steps of solution preparation, sample pretreatment, HPLC-ICP-MS condition and result determination, result calculation and the like. The determination method is convenient, rapid and accurate to implement.

A method for detecting a divalent cadmium ion in an aquatic product by using an HPLC-ICP-MS (High Performance Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometer) coupling technique belongs to the technical field of detection of aquatic products. The method comprises the following steps: 1), selecting instruments and equipment as well as an HPLC-ICP-MS coupling system; 2), configuring reagents and a standard solution; 3), processing a sample; 4), creating conditions for the experiment instruments; and 5), detecting the sample and calculating the results. According to the method, the cadmium in the aquatic product is extracted by neutral water in an ultrasonic way and the state of the cadmium is not changed, so that the cadmium in a free ion state and the cadmium subjected to complexation with organic matters such as protein both exist in the extract solution. In the adopted mobile phase, oxalate exerts a strong complexation effect on the cadmium ions but does not adsorb and elute stable cadmium complex in the extract solution, so that the cadmium ions and the cadmium complex in the sample can be guaranteed to be better separated. The method for detecting the divalent cadmium ion in the aquatic product by using the HPLC-ICP-MS coupling technique fills a blank in national standard that only the cadmium detection method is provided but no method for detecting the state of cadmium element is provided, therefore, the quality safety of the aquatic product and products of the aquatic product can be accurately and scientifically evaluated, meanwhile, the method is of great significance for formulating a new standard on the limit of harmful elements in the aquatic product.

The invention discloses methods for determining total amount arsenic and valence arsenic content in biological tissues and organs. The method comprises the following steps: 1) pretreatment, enzymolysis, filtration and decomposition are carried out on a biological tissues sample in order, and thereby arsenic is extracted; and 2) an ICP-MS method is used for determining the total amount arsenic content in the biological tissues sample. The invention also discloses a method for valence arsenic content in biological mechanism, the method comprises the following steps: 1) pretreatment, enzymolysis, and filtration are carried out on a biological mechanism sample in order, and thereby valence arsenic is extracted; and 2) a HPLC-ICP-MS method is used for determining the valence arsenic content in the biological mechanism sample. The method is simple and feasible, can effectively and completely extract the mercury in the biological mechanism, and can grantee the stability of the valence arsenic.

The invention discloses a method for detecting alkyl mercury in water based on a solid-phase extraction gathering and liquid-phase chromatograph-ICP-MS combined technology. The method comprises the following steps: a, gathering an alkyl mercury mixed standard series in a solid phase extraction manner; b, determining the gathered alkyl mercury mixed standard series by utilizing HPLC-ICP-MS to obtain a linear relation equation between the concentration of the standard series and an area of a chromatographic peak; c, gathering alkyl mercury in an unknown water sample in a solid-phase extraction manner; d, determining the gathered alkyl mercury of the unknown water sample by utilizing PLC-ICP-MS, substituting the obtained peak area into the linear equation, and calculating to obtain the concentration of the alkyl mercury in the water. By adopting the method, the linear detection range of the alkyl mercury is wide, and the detection limit is low. The method has characteristics of simplicity in operation, high accuracy, high sensitivity, high automation degree, environmental friendliness and the like and is suitable for determining alkyl mercury in surface water, water from sewage factories and water in water supply pipe network.

The invention discloses a method for determining the content of soluble mercury in cinnabar-containing drugs, characterized in the following steps: (1) that the soluble mercury is extracted from the cinnabar-containing drugs by an ultrasonic treatment and / or a magnetic stir with a bionic solvent; (2) that preferably a solution extracted in step (1) is purified; and (3) that an ICP-MS method is used to determine the content of the soluble mercury in the cinnabar-containing drugs. The invention also discloses a method for determining the content of soluble valence-state mercury in the cinnabar-containing drugs. In the invention the method for determining cinnabar drug effects and main toxicity components is established by simulating extraction manners in bodies and by adopting the ICP-MS method and an HPLC-ICP-MS method. In addition, the method is sensitive and accurate.