12 results about "Injection volume" patented technology

The invention provides a method for detecting related substances of sucrose octasulfate salt auxiliary materials, and particularly relates to the field of medicines. An SCX cation exchange chromatography filler and a C18 filler are mixed according to the ratio of (0.8-1.2): (3-5) to serve as a filling agent; the specification of a chromatographic column is CAPCELLPAK CR C18 + SCX 5 [mu] m, 250 * 4.6 mml.D.; 18-22 mM / L ammonium formate and 0.08-0.12% formic acid are used as a mobile phase A, and acetonitrile is used as a mobile phase B; a detector is CAD, the spray temperature is High, the collection frequency half-peak width is 0.1-0.2 min, the column temperature is 28-32 DEG C, the flow rate is 0.8-1.2 ml / min, and the sample injection volume is 4-6 [mu] l; wherein acetonitrile and water in a ratio of (3-5): (5-7) are used as diluents, and gradient elution is carried out; the method provided by the invention can effectively separate and accurately analyze each impurity, has strong specificity and good separation degree, and can effectively control the product quality.

The invention provides a detection method of black-bone chicken melanin oxidation products, and belongs to the technical field of chemical detection. The detection conditions of liquid chromatography in the detection method provided by the invention are as follows: the sample size is 0.9-1 [mu] L, a mobile phase A is a formic acid aqueous solution with the volume fraction of 0.05-0.15%, a mobile phase B is methanol, gradient elution is adopted, the detection time is 1-2 hours, and the detection wavelength is 250nm. The gradient elution conditions are as follows: the volume percentage content of the mobile phase B in 0-3 min is 5%-25%, the volume percentage content of the mobile phase B in 3-4 min is 25%-95%, the volume percentage content of the mobile phase B in 4-5.5 min is 95% B, the volume percentage content of the mobile phase B in 5.5-6 min is 95%-5%, and the volume percentage content of the mobile phase B in 6-8 min is 5% B. According to the present invention, the ultra-high performance liquid chromatography-mass spectrometry detection conditions are controlled, such that the detection accuracy is improved, the sample injection amount is reduced, the elution time is shortened, and the time and the sample consumption are saved.

The invention relates to the technical field of chemical gas chromatography analysis and detection, in particular to a device and method for chlorosilane detection, and the method comprises the following steps: inserting a needle head of an injector into a chlorosilane sample bottle, pulling back a push rod at a pulling-back speed of v, and extracting a sample of V1; the needle head of the injector faces upwards, bubbles float upwards to the top and are pushed and injected until the bubbles are discharged, and the needle cylinder is filled with the sample; according to the method, the needle head is inserted into a sample inlet of a heated gas chromatograph for detection, and the problem of inaccurate sample injection volume caused by bubbles generated by rapid volatilization of chlorosilane is effectively avoided through the steps of slow liquid extraction and bubble discharge, so that the accuracy of gas chromatography detection data and the repeatability of an experiment are remarkably improved; after the injection is finished, the specific high temperature of the sample inlet is combined, so that the chlorosilane sample is ensured to be instantly and completely gasified, the needle head is prevented from being remained or the sample is prevented from being volatilized in advance in the needle, the detection integrity is ensured, and the cross contamination of the sample inlet and a chromatographic column is avoided.

The present invention discloses an automatic injection device and a control system, and creatively proposes to improve the control system to precisely control the needle pushing, medicine pushing and the residence time of the needle under sufficient negative pressure, effectively reducing the occurrence of liquid leakage, effectively solving the technical problems of serious liquid leakage of the needle of the traditional injection device, resulting in poor stability of injection accuracy; there is a large deviation between the actual injection volume into the body and the target injection volume, and a large cumulative error is formed in subsequent injections; reducing the injection pain, effectively improving the treatment effect, and having a better customer experience.

The application discloses a detection method for determining the residual amount of easily hydrolyzed impurities in apremilast, which comprises the following steps: using a high performance liquid chromatograph, adopting polysaccharide derivatives as a filler (CHIRALPAK IH, 4.6mm*150mm, 5um), adopting a n-hexane-tetrahydrofuran (65:35) mobile phase, a flow rate of 1.0ml per minute, a column temperature of 30 DEG C, a detection wavelength of 230nm, and a sample injection volume of 50ul. The application adopts the polysaccharide derivative filler to determine the easily hydrolyzed impurities in the apremilast, has high separation efficiency, strong anti-interference ability, fast analysis speed and high detection sensitivity, and can effectively control the quality of the apremilast by determining the amount of the easily hydrolyzed impurities in the apremilast.

The invention discloses a method for detecting the hydrazine content in a lamotrigine key intermediate. The method comprises the following steps: respectively dissolving a test sample and a reference substance in a detection solvent to obtain a test sample solution and a reference substance solution; respectively separating the test solution and the reference substance solution by adopting a liquid chromatography technology, detecting by adopting a mass spectrometry detector, and calculating the content of hydrazine by adopting an external standard method according to a peak area; the liquid chromatography conditions are as follows: a C18 chromatographic column is adopted, and the flow rate is 0.5-0.7 ml / min; the column temperature is 30-40 DEG C; the sample size is 10 microliters; the mobile phase is A: 0.1% formic acid aqueous solution; b: acetonitrile; 8%-12% of A and 92%-88% of B are used for isocratic elution; the mass spectrometry conditions are as follows: in an ESI + positive ion mode, the taper hole voltage is 52V, the parent ion m / z is 113.3, the quantitative ion pair m / z is 113.3 / 56.4, the quantitative ion collision energy is 14V, the qualitative ion pair m / z is 113.3 / 58.4, and the qualitative ion collision energy is 15V. The methodology verifies that the method is suitable for quantitative detection of the hydrazine content in the lamotrigine key intermediate.

The invention discloses a high-pressure sampling method for gas chromatographic analysis. The method comprises the following steps: (1) collecting a sample through a sampling steel cylinder; the sample steel cylinder is connected with the quantitative sample injection valve through the switching valve; (2) cleaning a solvent cavity and a sample injection cavity of the quantitative sample injection valve by using a solvent through a cleaning pipeline, and purging the cleaned solvent to a vaporizing chamber through a GC system carrier gas and a sample injection needle; then quantitatively filling the sample injection cavity and the solvent cavity with the solvent again; (3) purging the sample injection cavity by using inert gas through the purging pipeline, wherein the solvent is continuously reserved in the solvent cavity in the purging process; (4) opening an inlet / outlet valve of the sampling steel cylinder, and quantitatively filling the sample into the sample injection cavity; and (5) sequentially blowing the sample in the sample injection cavity and the solvent in the solvent cavity into a vaporizing chamber through a sample injection needle by virtue of GC system carrier gas, and entering a chromatographic column for gas chromatographic analysis. According to the invention, the problem of sample injection distortion can be thoroughly solved, and the consistency and fidelity of the sample injection amount are ensured.

The utility model relates to the technical field of sample injection volume measurement of an ion chromatograph, in particular to a sample injection volume measurement device of the ion chromatograph, which comprises a sample injection volume controller, two water passing ports are fixedly arranged on the side surface of the sample injection volume controller, one side of each water passing port is fixedly provided with a water passing pipe, one side of each water passing pipe is provided with a fixed pipe, and the other side of each water passing pipe is provided with a fixed pipe. Sealing pipes are arranged in the two fixing pipes, first sealing rings are arranged on the side faces of the two sealing pipes, second sealing rings are arranged on one sides of the two fixing pipes, two mounting bases are fixedly arranged on the side faces of the two fixing pipes, positioning plates are fixedly arranged on one sides of the four mounting bases, and two connecting boxes are fixedly arranged on the side faces of the two water passing pipes; the utility model has the beneficial effects that the liquid inlet pipe and the liquid outlet pipe are convenient to disassemble and assemble, so that the liquid inlet pipe and the liquid outlet pipe are convenient to replace and clean, the influence on the sample injection flow due to blockage of the liquid inlet pipe and the liquid outlet pipe is avoided, and the accuracy of a detection result is improved.

The invention relates to a carbetocin injection isomer detection method, and belongs to the technical field of polypeptide drug impurity analysis. The carbetocin injection isomer detection method comprises the following steps: detecting Ile position isomer impurities in 8-site Leu in a carbetocin raw material by adopting a high performance liquid chromatography; the adopted chromatographic conditions are as follows: octadecyl silane bonded silica gel is taken as a filling agent, acetonitrile-0. 02 mol / L ammonium acetate-0.03 mol / L monopotassium phosphate is taken as a mobile phase A, methanol-acetonitrile is taken as a mobile phase B, and gradient elution is performed; the detection wavelength is 210 to 230 nm; the column temperature is 40-70 DEG C; the flow velocity is 0.5 to 1.2 mL / min; and the sample injection volume is 10-40 [mu] L. The carbetocin injection isomer detection method is high in accuracy and good in sensitivity, repeatability and precision meet requirements, position isomer impurities can be accurately detected, and the product quality can be better controlled.

A liquid injection device, a liquid injection method, and a microfluidic system are disclosed. The liquid injection device (100) has an injection mode and a replenishment mode. In the injection mode, a transmission liquid is injected into the first cavity (111), which acts on the first surface (311) and drives the second sliding part (32) to slide through the first connecting part (33), so that the reaction liquid in the fourth cavity (212) or the downstream section of the fourth cavity (212) is injected into the reaction device (200). In the replenishment mode, a transmission liquid is injected into the second cavity (112), which acts on the second surface (312) and drives the second sliding part (32) to slide through the first connecting part (33), so that the reaction liquid injected into the fourth cavity (212) or the downstream section of the fourth cavity (212) is contained therein. The area of ​​the transmission liquid acting on the first surface (311) is larger than the area of ​​the transmission liquid acting on the second surface (312), so slow injection and rapid replenishment can be achieved. Slow injection is beneficial for precise and micro-control of the injection volume.

This invention relates to a method for determining the encapsulation efficiency of liposome injection solutions. The method comprises the following steps: 1) preparation of a blank solution; 2) preparation of a test solution; 3) determination: injecting the blank solution and the test solution into a high-performance liquid chromatograph (HPLC) to obtain a chromatogram, and calculating the encapsulation efficiency of the test solution based on the peak area of ​​the chromatogram. The chromatographic conditions for the HPLC are as follows: instrument: HPLC system, VWD or DAD; column: Thermo Hypersil BDS C8; mobile phase: sodium hexanesulfonate solution: acetonitrile = 75:25; column temperature: 40℃; flow rate: 1.0 ml / min; detection wavelength: 255 nm; injection volume: 10 μl; run time: 10 min.

The invention relates to the technical field of drug analysis, and discloses a method for determining impurity I in bumetanib injection, which comprises the following steps: using a reverse high performance liquid chromatograph and an ultraviolet detector, taking ACE Excel C18-PFP as a chromatographic column, taking 0.1% phosphoric acid aqueous solution as a mobile phase A, taking methanol-acetonitrile (40: 60) as a mobile phase B, adopting a gradient elution procedure, and determining the impurity I in the bumetanib injection according to the detection wavelength of 220nm, the sample injection volume of 10mu L and the flow velocity of 1.0 mL / min. The column temperature is 30 DEG C; the content of the impurity I in the bumetanib injection can be accurately detected, the blank of no impurity I detection method report is filled, and method verification is carried out. The method designed by the invention can be used for separating and accurately determining the impurity I in the bumetanib injection, and is high in specificity, high in sensitivity and good in precision and accuracy; and the quality control of the bumetanib injection is effectively enhanced.