129 results about "Column temperature" patented technology

The invention relates to a chromatographic instrument temperature control method and system, an intelligent terminal and a storage medium, and relates to the technical field of chromatographic instrument sample separation.The method comprises the steps that the sample type of a preset sample is obtained; analyzing the sample type to determine a window heating rate and a window target temperature; acquiring a chromatographic column initial temperature of a preset chromatographic column; analyzing the initial temperature of the chromatographic column and the target temperature of the window to determine the temperature of the chromatographic column needing to be increased; analyzing the temperature required to be increased and the window heating rate of the chromatographic column so as to determine the heating time of the chromatographic column; and controlling a preset chromatographic column temperature regulation and control device to perform temperature control on the chromatographic column according to the chromatographic column heating time and the window target temperature. The method has the effect of improving the precision of the temperature retention time.

The invention discloses an independent liquid chromatography column oven, and relates to the technical field of column ovens, the independent liquid chromatography column oven comprises a column oven body, the inner side of the column oven body is fixedly connected with a plurality of separation frames, the inner sides of the separation frames are fixedly connected with supporting blocks, the outer sides of the supporting blocks are provided with liquid chromatography columns, and the liquid chromatography columns are arranged on the outer sides of the liquid chromatography columns. Connectors are fixedly connected to the left end and the right end of the liquid chromatographic column, a mounting unit for mounting the liquid chromatographic column is arranged on the inner side of the separation frame, and a fixed cover and a pump body are fixedly connected to the left side of the column oven body. According to the column oven for the independent liquid chromatography, a plurality of separation frames are arranged, a plurality of chromatographic columns are contained, the same instrument and multi-item convenient switching detection are facilitated, and through a guide plate, a guide block, a fixing rod, an installation box, a rotating pipe, installation heads, a second gear piece, a toothed plate and an electric push rod, the installation heads on the left side and the right side are conveniently controlled to rotate and get close to each other; and the liquid chromatographic column is quickly connected with the pump body, so that the workload of workers is reduced, and the operation is simple.

The invention relates to the technical field of food safety detection, in particular to a method for detecting urea in bean sprouts and application thereof.The method comprises the following steps that smashed bean sprouts are subjected to two times of ultrasonic extraction and centrifugation, supernate is combined, and an extracting solution is obtained; fixing the volume and filtering to obtain a to-be-detected solution; detecting the liquid to be detected by using liquid chromatography-tandem mass spectrometry; an extraction solvent for ultrasonic extraction is a 5% formic acid-acetonitrile composite solution; the conditions of the liquid chromatography-tandem mass spectrometry are as follows: the chromatographic conditions are as follows: a chromatographic column is an HILIC column; the sample size is 10 [mu] L; a mobile phase is a mixed solution of a 0.02 mmol / L ammonium acetate buffer salt solution and acetonitrile, and isocratic elution is carried out; the flow rate is 0.3 mL / min; the column temperature is 40 DEG C; mass spectrum conditions are as follows: an electrospray ionization (ESI) positive ion mode, electrospray voltage of 4000 V, sheath gas pressure of 30 psi, auxiliary gas pressure of 5 psi, capillary heating temperature of 300 DEG C and scanning mode of MRM. The method disclosed by the invention is free from substance interference, high in sensitivity, accurate in result, low in cost and high in efficiency, and can be used as a standard detection method.

The invention discloses a method for simultaneously detecting 37 phenolic substances in a plant based on HPLC (High Performance Liquid Chromatography). HPLC-PDA (Personal Digital Assistant) is adopted for separation and detection; the detection conditions are as follows: the chromatographic column is a PFP chromatographic column; the detection wavelengths are 280 nm, 330 nm and 360 nm; the flow velocity is 0.5 to 0.8 mL / min; the sample size is 8-12 [mu] L; the column temperature is 28-32 DEG C; the mobile phase A is an aqueous solution containing 0.3% by mass of formic acid, and the mobile phase B is methanol; the elution gradient is 0-10 min, and the elution gradient is 5-10% B; in 10-16 min, 10%-25% of B is obtained; after 16 to 25 minutes, 25 to 40 percent of B is obtained; 25 to 50 minutes, 40 to 60 percent of B is adopted; and 60-67% of B is carried out in 50-55 min. The method is suitable for plant sample detection, is especially suitable for sea-buckthorn sample detection, can be applied to multiple fields of food analysis, plant research, component development and the like, and has wide application value.

The invention relates to the technical field of chemical detection, and particularly discloses a method for detecting impurities in propafenone hydrochloride injection. The invention discloses a method for detecting impurities in propafenone hydrochloride injection, which comprises the following steps: detecting a sample to be detected by using high performance liquid chromatography to obtain the content of the impurities, in the detection process, octadecylsilane chemically bonded silica is used as a filling agent of a chromatographic column; the column temperature is 28-32 DEG C, and the flow velocity is 0.8-1.2 ml / min; the mobile phase comprises a mobile phase A and a mobile phase B, the mobile phase A is 0.012-0.017 mol / L dipotassium phosphate solution, and the pH value of the mobile phase A is adjusted to 2.2-2.8 with phosphoric acid; and the mobile phase B is acetonitrile. The detection method provided by the invention is simple to operate and high in detection speed, and has the advantages of high sensitivity, high precision, high repeatability and high accuracy.

The invention belongs to the technical field of separation and detection, and particularly relates to a method for determining iodide in domestic drinking water. Measuring the iodide in the domestic drinking water by adopting a high performance liquid chromatography-ultraviolet detection method; taking a domestic drinking water sample solution for detection, and quantifying by an external standard method; according to the detection method, a Metrosep A Supp5-250 chromatographic column (250 mm * 4.0 mm, 5 [mu] m) is adopted for separation, 4.5 mmol / L Na2CO3, 1.0 mmol / L NaHCO3 and 35% acetonitrile are adopted as a mobile phase, a DAD detector is adopted, the wavelength is 226 nm, the flow rate is 0.60 mL / min, and the column temperature is 50 DEG C. The invention also discloses a method for detecting the content of the sodium hydroxide in the sample. According to methodology verification, the method can be used for measuring iodide in domestic drinking water, the detection limit is 2.0 mu g / L and is superior to that of a spectrophotometric method and a volumetric method in the national standard, no complex pretreatment process exists, specificity is high, toxic and harmful chemical reagents are not used, online automatic sample injection can be achieved, and the method has obvious advantages for large-batch samples; compared with inductively coupled plasma mass spectrometry, used instruments are relatively cheap, and basic popularization and application are facilitated.

This utility model relates to a column housing device for housing a chromatographic column within a column oven. The device includes: a housing with a base having a first side and an opposite second side, wherein the first side has a groove; a first sidewall and a second sidewall extending from the first side of the base, wherein the second sidewall is arranged opposite to the first sidewall; and a support member including a bracket disposed in the groove, such that the support member is detachably fixed to the first side of the base via the bracket between the first and second sidewalls, thereby forming a heat exchange channel between the base, the support member, and the first and / or second sidewalls for placing the chromatographic column. This column housing device detachably connects the support member to the housing, providing a flexible and adjustable thermal structure that balances column placement stability and heat transfer efficiency. This utility model also relates to a column oven and a chromatogram.

The invention provides a system and method for detecting the content of a corrosion inhibition additive in cooling liquid, specifically, the system comprises a liquid chromatograph, a diode array detector DAD and an electric fog detector CAD which are sequentially connected in series, the liquid chromatograph comprises a mobile phase pump, an automatic sampler and a column oven, and a chromatographic column is arranged in the column oven; wherein the mobile phase pump is used for mixing different mobile phases according to a preset proportion and then conveying the mixed mobile phases to the automatic sample injector; the automatic sample injector is used for injecting the mobile phase from the mobile phase pump into the to-be-detected cooling liquid and flushing the to-be-detected cooling liquid injected with the mobile phase to the chromatographic column; the column oven is used for controlling the column temperature of the chromatographic column; the chromatographic column is used for performing chromatographic separation on the corrosion inhibition additive in the to-be-detected cooling liquid; the DAD is used for detecting the corrosion inhibition additive containing the benzene ring in the cooling liquid to be detected; the CAD is used for detecting the polybasic aliphatic carboxylic acid type corrosion inhibition additive in the cooling liquid to be detected.

The application relates to the technical field of data processing, and provides a method for calculating a temperature field, which comprises the following steps: determining a first density of first column temperature sampling points; determining the number A of temperature sampling points between a first temperature sensor and a second temperature sensor according to a first interval between the first temperature sensor and the second temperature sensor and the first density; determining A temperature values through interpolation operation according to temperature values of the first temperature sensor and the second temperature sensor; determining a second density of first row temperature sampling points; determining the number B of temperature sampling points between the first temperature sampling points and the second temperature sampling points according to a second interval between the first temperature sampling points and the second temperature sampling points and the second density; determining B temperature values through interpolation operation according to temperature values of the first temperature sampling points and the second temperature sampling points; and determining the temperature field of a machine room according to the A temperature values and the B temperature values. The method can improve the efficiency of calculating the temperature field.

The invention relates to a method for analyzing and detecting a non-azonetin enantiomer, which adopts normal-phase high performance liquid chromatography and takes normal hexane-ethanol-trifluoroacetic acid as a mobile phase to detect the non-azonetin enantiomer, and the specific chromatographic conditions are as follows: a chromatographic column is prepared by covalently bonding amylose-tri (3, 4, 6-trimethyl-1, 3-pentanediol) on the surface of silica gel; 2, 5-dichlorophenyl carbamate is used as a filling agent (IE, 4.6 * 250 mm, 5.0 [mu] m); a mobile phase: n-hexane: ethanol: trifluoroacetic acid = 500: 500: 1 (V / V / V); the flow rate is 1.0 ml / min; the column temperature is 30 DEG C; the sample size is 20 [mu] l; the detection wavelength is 280 nm; the elution gradient is isocratic elution. The invention provides a high performance liquid chromatography method for analyzing the enantiomer of the fiazonetin, the complete separation of the fiazonetin and the enantiomer of the fiazonetin can be realized by adopting the method, and the separation degree of a main component and the enantiomer is greater than 1.5.

The invention relates to the technical field of biological analysis, in particular to a fish and crustacean biological analysis device which comprises a placing frame and a mobile phase solvent bottle placed in the upper portion of the placing frame, a vacuum degassing box is connected to the lower portion of the placing frame, and a high-pressure pump box is connected to the lower portion of the vacuum degassing box. A sample injection box is connected to the lower part of the high-pressure pump box, a detection box is connected to the lower part of the column oven, an automatic sample injector is arranged in the sample injection box above the placing frame, and a chromatographic column is connected to the interior of the column oven. According to the biological analysis device for the fishes and the crustaceans, through slight shaking in multiple directions, the uniform shaking efficiency and effect of a sample solution in the sample solvent bottle can be improved, the situation that particles settle to the bottom of the bottle and are layered due to long-time standing of the sample solvent bottle is avoided, the concentration of the sample solution sucked by an automatic sample injector is uniform, and the accuracy of the sample solution is improved. Therefore, the accuracy of the detection result of the biological analysis device can be improved, and the biological analysis work of fishes and crustaceans cannot be influenced.

The utility model discloses a column temperature box with automatic chromatographic column selection system, including the box, the box surface is equipped with the door body of rotation connection, is equipped with the valve cut system in the box to the door body one side, and the valve cut system includes the mounting panel in the box top, the chromatographic column installation valve head on the mounting panel, the control valve in the chromatographic column installation valve head tail portion, is equipped with the temperature control area below the valve cut system, and the temperature control baffle that installs in the box is equipped in the temperature control area, and the mounting bracket on the surface of temperature control baffle and the chromatographic column on the mounting bracket, the bottom of temperature control area still is equipped with the liquid leakage device.

The invention discloses a method for detecting 5 '(E)-VPA phosphoramidite monomer related substances, and belongs to the technical field of liquid chromatography detection. Related substances comprise 5 '-(E)-VP-2'-OMe-A (Bz), 5 '(Z)-VPA, 5'-(E)-VP-2 '-OMe-A-CE-P and 5' (E)-VPA-OX, and chromatographic detection conditions comprise that the column temperature is 23-27 DEG C, a stationary phase of a chromatographic column is octadecyl bonded silica gel, a mobile phase A is an ammonium acetate solution, a mobile phase B is acetonitrile, gradient elution is performed, and the like. According to the method, four related substances in the 5 '(E)-VPA phosphoramidite monomer are effectively separated through specific liquid chromatography conditions, the system adaptability, specificity, linearity and range, detection limit, quantitation limit and accuracy verification of the method all meet acceptable standards of pharmacopoeia, and detection of multiple related substances can be completed within a short time; and a reliable means is provided for detecting and controlling the quality of the 5 '(E)-VPA phosphoramidite monomer.

The invention belongs to the technical field of analysis and testing, and particularly relates to a method for measuring the optical purity of L-lactide. The method comprises the following steps: taking a CHIRALP AK-H chiral column as a chromatographic column; n-hexane-isopropanol is used as a mobile phase; the column temperature is 25-35 DEG C; the detection wavelength is 208 to 212nm; the method provided by the invention has the advantages that the sample introduction volume is 20 [mu] l, effective separation and quantitative detection of meso-lactide, L-lactide and D-lactide are realized, the detection result is accurate and reliable, and a basis is provided for quality control of L-lactide.

The invention belongs to the technical field of gas chromatography detection, and relates to a gas chromatography method for simultaneously determining the content of ethanol and isopropyl myristate. The set conditions of the gas chromatography are as follows: the temperature of an FID detector and a polyethylene glycol 20M capillary column is 240-260 DEG C, the temperature of the detector is 240-260 DEG C, the carrier gas is nitrogen, the flow rate is 0.9-2.5 mL / min, the sample injection amount is 1 mu L, the column temperature is increased by adopting a program, the initial temperature is 80-90 DEG C, the temperature is increased to 180-190 DEG C at the rate of 9-12 DEG C / min, and the temperature is maintained for at least 10 minutes. The method provided by the invention can realize simultaneous detection of ethanol and isopropyl myristate, after the two substances are dissolved by the N, N-dimethylformamide solvent, the detected spectrogram does not have the phenomena of peak overlapping, trailing and the like, and the method has the advantages of high separation efficiency, high selectivity, high sensitivity, high analysis speed and wide application range.

The invention discloses a method for determining the content of poloxamer 124 in the technical field of medical analysis. Liquid chromatography is adopted for detection, and a gel chromatographic column filled with porous silicon dioxide is selected as a chromatographic column; a mobile phase is a trifluoroacetic acid-acetonitrile-water solution; the weight ratio of the mobile phase trifluoroacetic acid to acetonitrile to water is 0.1: (18-22): (78-82); the column temperature is 25-45 DEG C; the temperature of a detector is 60-80 DEG C; the flow velocity of the mobile phase is 0.6-1.0 ml / min; the sample size is 5-20 [mu] l, automatically injecting the sample according to the chromatographic conditions, recording the peak area, and calculating the content according to an area normalization method. The method is high in response value, simple in detection operation and high in product content accuracy, specificity, repeatability, sampling precision, linearity and range all meet the requirements, and the quantitative determination problem of poloxamer 124 is solved.

The present invention provides a method for simultaneously determining 5-hydroxymethylfurfural and its oxidation product, including: providing a reaction mixture obtained after 5-hydroxymethylfurfural is oxidized, the reaction mixture comprising 5-hydroxymethylfurfural and its oxidation product; filtering the reaction mixture to obtain a filtrate and a filter residue; preparing the filtrate as a first solution to be tested, mixing the filter residue with an inorganic base so that the insoluble oxidation product in the filter residue undergoes a salt-forming reaction and dissolves, and preparing the filtrate as a second solution to be tested; performing high performance liquid chromatography analysis on the first solution to be tested and the second solution to be tested, respectively, the conditions for high performance liquid chromatography analysis comprising: an organic acid analytical column as the stationary phase, and a column temperature of 25°C to 60°C; an inorganic acid aqueous solution as the mobile phase, and a flow rate of the mobile phase of 0.4 to 1 mL / min; an injection volume of 1 μL to 20 μL; and adopting dual wavelength detection, with a first detection wavelength of 200 nm to 240 nm and a second detection wavelength of 250 nm to 300 nm. The method provided by the present invention has good separation, high accuracy, and high precision.

The present invention discloses a stand-alone column temperature box for liquid chromatography, which relates to the technical field of column temperature boxes and includes a column temperature box body, wherein a plurality of partition frames are fixedly connected to the inner side of the column temperature box body, a support block is fixedly connected to the inner side of the partition frame, a liquid chromatography column is arranged on the outer side of the support block, the left and right ends of the liquid chromatography column are fixedly connected with connectors, the inner side of the partition frame is provided with an installation unit for installing the liquid chromatography column, and the left side of the column temperature box body is fixedly connected with a fixed cover and a pump body. The stand-alone column temperature box for liquid chromatography, by being provided with a plurality of partition frames, can accommodate a plurality of chromatography columns, so that the same instrument can conveniently switch and detect multiple projects, and through the guide plate, guide block, fixed rod, installation box, rotating tube, installation head, gear part 2, tooth plate and electric push rod, it is convenient to control the installation heads on the left and right sides to rotate and approach each other, so that the liquid chromatography column can be quickly connected to the pump body, reducing the workload of the staff and simplifying the operation.

The invention provides a method for determining D-psicose in processed food and application of the method. The method specifically comprises the following steps: extracting a sample with warm water at 50-60 DEG C, precipitating protein by adopting a Carrez reagent, and removing interference impurities; chromatographic conditions are defined as follows: a calcium type strong cation exchange column is adopted, pure water containing 50 mg / L of EDTA-Ca is adopted as a mobile phase, the flow rate is 0.4-0.6 mL / min, and the column temperature is 80 DEG C. The result shows that the linear relation of the D-psicose is good in the concentration range of 1.0 mg / mL to 20.0 mg / mL, and the correlation coefficient is 0.999999; according to the method, the LOD is 0.002 g / 100g, and the LOQ is 0.005 g / 100g. Under the experimental conditions of standard addition before simulation processing, the average recovery rate of 18 matrixes including dairy products, bakery products and the like is 81.5-128.1%, and the RSD is less than 3.0%. The determination method provided by the invention is simple in pretreatment, high in sensitivity, strong in interference resistance and good in accuracy, effectively solves the ubiquitous problems of matrix wrapping, matrix interference, difficulty in isomer separation and the like when the D-psicose in the processed food is detected, can realize rapid and accurate detection of the D-psicose in all dosage forms of processed food, and has a wide prospect.

The invention discloses a method for improving the detection recovery rate of ascorbyl palmitate in a compound product, which comprises the following steps: taking a sample, adding BHT (butylated hydroxytoluene), then adding an isopropanol-n-hexane mixed solution containing 0.8-1.2% by volume of glacial acetic acid as an extraction solvent, then fully mixing, extracting, freezing, centrifuging, taking supernate, and collecting the supernate to obtain the ascorbyl palmitate. The chromatographic conditions are as follows: a C18 reversed-phase chromatographic column is adopted, a mobile phase A and a mobile phase B are used for gradient elution, the flow velocity of the mobile phase is 0.8-1.2 mL / min, the column temperature is 28-32 DEG C, and the maximum absorption wavelength of ascorbyl palmitate is taken as the detection wavelength. According to the method, the extraction efficiency is improved by optimizing a sample pretreatment process, and the problem that the liquid phase detection error of the substance in the compound product is generally higher than 10% is effectively solved in combination with improved high performance liquid chromatography separation conditions.

The invention relates to the technical field of analytical chemistry, in particular to an analytical method of 1, 2, 3-tri (2-cyanoethoxy) propane, which adopts gas chromatography for detection, and adopts a hydrogen flame ionization detector as a detector; the capillary chromatographic column is a weak-polarity column or a medium-polarity column; the temperature of a hydrogen flame ionization detector is 300-350 DEG C; the temperature of a sample inlet is 200-250 DEG C; the column temperature of a capillary gas chromatographic column is firstly set to be 40-80 DEG C, the holding time is 5-10 min, then the temperature is increased to 250-300 DEG C at the speed of 10-15 DEG C / min, and the holding time is 20-30 min; the carrier gas is nitrogen or helium. The analysis method is low in operation cost, the chromatographic column has good thermal stability, the peak shape, the separation degree and the repeatability are better, the accuracy is higher, and the method has the characteristics of rapidness, simplicity, accuracy and the like.

The present invention relates to the technical field of detection systems, in particular to a system for detecting the content of N-bromosuccinimide in sodium sugammadex. The system comprises a chromatograph main body for elution and separation and a mass spectrometer main body for detection, wherein a column oven is connected between the chromatograph main body and the mass spectrometer main body, and a chromatographic column for sample elution and separation is assembled in the column oven; a liquid inlet seat and a liquid outlet seat are provided in the column oven, respectively communicating with the chromatograph main body and the mass spectrometer main body, and the chromatographic column is positioned and assembled between the liquid inlet seat and the liquid outlet seat; a telescopic joint structure is provided at the end of the chromatographic column, the chromatographic column is connected to the liquid inlet seat and the liquid outlet seat via the joint structure, and a glass wool column can be positioned and loaded in the joint structure; a combined water bath structure is provided in the column oven based on an inner partition, and the assembled water bath structure can seal the chromatographic column main body structure; the present invention can achieve the purpose of improving the accuracy of content detection.

The invention discloses a method for preparing chimonanthine from chimonanthus praecox seeds. In the high-speed counter-current chromatography separation process, the two-phase solvent system adopts hexane-ethyl acetate-methanol-water with the volume ratio of 3: 5: 3: 5, the upper layer is used as a stationary phase to be pumped into a counter-current chromatography separation column, the lower layer is used as a mobile phase to be pumped into a high-speed counter-current chromatograph for counter-current extraction separation, the rotating speed of a main machine is 800r / min, the flow velocity of the mobile phase is 2mL / min, the column temperature is 30 DEG C, and the volume ratio of hexane to ethyl acetate to methanol to water is 3: 5: 3: 5; and collecting the target component, carrying out reduced pressure distillation to remove the solvent to obtain chimonanthine with the purity of 84.6%, and further recrystallizing to obtain a reference substance with the purity of 96.5%. The method has the advantages of low cost, simple process, high purity, quick separation and purification and easiness in preparation.

The present invention discloses a method for constructing a characteristic spectrum of Trillium gracile for distinguishing Trillium gracile and its processed products and counterfeits, and its application. By optimizing column temperature and flow rate, optimizing chromatographic columns and other conditions, the present invention allows the Trillium gracile characteristic spectrum to contain more information, with a more stable baseline and better chromatographic peak separation. Through multi-batch testing, common peaks are selected and identified using reference substances. On this basis, Trillium gracile and Trillium gracile can be quickly distinguished through different chromatographic peaks. Simultaneously, through mathematical and statistical analysis, characteristic peaks that can distinguish Trillium gracile from vinegar Trillium gracile slices are optimized, and relative peak areas are optimized, providing a rapid and information-rich characteristic spectrum construction method for quality control analysis of distinguishing Trillium gracile from vinegar Trillium gracile slices.

The invention relates to the technical field of polypeptide detection, in particular to a method for detecting the content of a semeglutide polymer. A liquid chromatography method is adopted, wherein a chromatographic column is G2000 SWxl; carrying out isocratic elution for 40 minutes; the detection wavelength is 280 nm; the column temperature is 26-30 DEG C; the mobile phase is formed by mixing a phosphate solution of sodium chloride and isopropanol according to the volume ratio of 50: 50. The selected mobile phase has no influence on the retention performance of the chromatographic column, the separation degree of the polymer and the main peak is greater than 1.5, and the requirement on an instrument is lower; accurate and reliable experimental results can be obtained by determining the polymer in the semeglutide through the method.

The invention belongs to the field of fruit quality analysis, and particularly relates to a high performance liquid chromatography method for simultaneously determining organic acid and vitamin C in kiwi fruit, which comprises the following steps: grinding kiwi fruit into powder in liquid nitrogen, extracting with metaphosphoric acid solution, centrifuging, and collecting supernate to obtain test solution; a high performance liquid chromatograph is utilized, and under the chromatographic conditions that a C18 column is selected as a chromatographic column, the column temperature is 25-35 DEG C, the sample injection volume is 10 microliters, a 0.01 mol / L monopotassium phosphate buffer solution is used as a mobile phase for isocratic elution, and the organic acid and the vitamin C in a test solution are detected under the conditions that the flow speed is 0.5-0.8 mL / min and the wavelengths are 210 nm and 245 nm. The detection method provided by the invention can realize qualitative and quantitative analysis of flavor and nutritional ingredients of kiwi fruits, and has good specificity, accuracy, durability and stability and high detection sensitivity.

The invention belongs to the technical field of pharmaceutical analysis, and discloses a liquid chromatography detection method of a pimobendan intermediate, which comprises the following steps: injecting octadecyl bond and silica gel as a stationary phase, a phosphate buffer solution with the pH value of 3.0-5.0 as a water phase and methanol (or acetonitrile) as an organic phase into a high performance liquid chromatograph under the conditions that the column temperature is 30-60 DEG C, the sample injection is 5-30 mu L and the flow velocity is 0.5-2 ml / min, and carrying out gradient elution to obtain the pimobendan intermediate. And the sample is analyzed in a wavelength range of 200-230nm. By adjusting the mobile phase system and optimizing the mobile phase gradient, a main peak and an impurity peak are completely separated, the analysis speed is high, the detection sensitivity is high, and the stability and the quality of a product in production can be better detected.

The invention relates to the technical field of drug analysis and detection, and provides a method for detecting 1, 2, 4-triazole in fluconazole sodium chloride injection, which adopts high performance liquid chromatography. The specific conditions of the high performance liquid chromatography are as follows: a solvent is a water-acetonitrile mixed solution with the volume ratio of 95: 5; the mobile phase comprises a mobile phase A and a mobile phase B, the mobile phase A is water, and the mobile phase B is acetonitrile; the flow velocity is 1.0 mL / min; octadecylsilane chemically bonded silica is used as a filling agent of a chromatographic column; the column temperature is 30 DEG C; the sample injection volume is 100 microliters; performing gradient elution; and the detection wavelength is 195 nm. The method has the advantages that the content of 1, 2, 4-triazole in the fluconazole sodium chloride injection can be quantitatively and accurately determined without derivation reaction, the unification of operation convenience and detection accuracy is realized, and reliable technical support is provided for quality control of the fluconazole sodium chloride injection.

The application discloses a method for improving the chromatographic separation degree of impurities A and B in acetylcysteine raw materials, and is characterized by the following steps: controlling the column temperature of a chromatographic column within a specific low temperature range of 15 DEG C plus or minus 2 DEG C, and using the difference between the distribution behaviors of impurities A and B between a stationary phase and a mobile phase at different temperatures to significantly improve the separation degree of the two impurities. When the column temperature is 15 DEG C, the separation degree of impurities A and B can reach 2.06, which is much higher than the pharmacopoeia standard, and the separation degrees under the conditions of 30 DEG C, 35 DEG C and 40 DEG C all fail to meet the standard. The application does not need to replace the chromatographic column, is simple and convenient to operate, low in cost, can stably meet the accurate quantification requirements of related substances in acetylcysteine raw materials, and has good popularization and application value.

The present application discloses a method for simultaneously detecting multiple sugars and sugar alcohols, comprising the following steps: 1) preparing a sample solution to be detected; 2) using ultra-high performance liquid chromatography-mass spectrometry to qualitatively or quantitatively detect sugars and sugar alcohols in the sample solution to be detected; wherein, the chromatographic separation conditions of the ultra-high performance liquid chromatography-mass spectrometry are: chromatographic column: Waters Acquity BEH Amide 2.1×100mm; column temperature: 10°C; flow rate: 0.2-0.5 mL / min; injection volume: 0.1-1 μL; mobile phase: phase A is 0.1% formic acid water, phase B is acetonitrile, and gradient elution is performed. The present application can simultaneously detect ten sugars and sugar alcohols, and can also simultaneously detect isomers of multiple sugars, with very high sensitivity.