Overview
Chromatographic methanol is a chromatographic grade reagent of methanol, used for chromatographic analysis, chromatographic separation, and chromatographic preparation.
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CN201510000448 discloses a method for separating and purifying tartirelin by combining low-pressure preparative chromatography and high-pressure liquid phase preparative chromatography. It mainly solves the technical problem that the existing technology cannot obtain high-yield products. The separation and purification method of the present invention includes the following steps:
1) Treat the crude liquid peptide obtained by solid-phase synthesis with diethyl ether first, remove the cutting liquid inside, and then add deionized water for layering to obtain the supernatant liquid as a crude liquid. Repeat the water washing and layering many times to obtain a crude liquid. Liquid;
2) Use chromatographic methanol (or ethanol) aqueous solution to filter the crude liquid with a conventional column vacuum column chromatography device to obtain a product with a purity of more than 95%, and then use a reversed-phase silica gel water-based short column; the mobile phase is two-phase, acetic acid The aqueous solution is phase A, and the chromatographic methanol (or ethanol) aqueous solution is phase B. Perform gradient elution and purification to collect the peptide solution with the target peak;
3) The obtained peptide solution is concentrated and freeze-dried by rotary evaporation under reduced pressure;
4) Reprocessing: Add diethyl ether to precipitate 2-5 times to the freeze-dried product to obtain acetate-containing powdered product. Through the present invention, acetate-containing tartirelin with a purity greater than 99% can be obtained.
CN201710159438 discloses a quantitative detection method for abiraterone in whole blood. Whole blood is used as the test object, and the following steps are performed in sequence: add ethyl acetate to the whole blood lysate, vortex, centrifuge, and ethyl acetate. Blow dry the layer with nitrogen flow, redissolve it with 20% acetonitrile aqueous solution, and centrifuge to absorb the supernatant I; weigh the alkaline diatomite and put it into a glass chromatography column, shake it, and then add the supernatant I and add pure water in sequence. , 20% methanol aqueous solution, chromatographic methanol elution, the eluate was blown dry by nitrogen flow, reconstituted with 20% acetonitrile aqueous solution, and centrifuged. The supernatant II was absorbed for high-performance liquid chromatography system analysis, and the abiraterone drug peak area Y was obtained. , substitute into the formula Y=27524X+1956.6, X is the abiraterone concentration of the supernatant II; then after conversion, the abiraterone concentration in the whole blood to be measured is obtained.
CN201110429196 discloses a HPLC-MS-MS detection method for chloramphenicol residues in functional foods, which includes the following steps: weigh the sample, add deuterated chloramphenicol as an internal standard solution, add ethyl acetate, hydrogen Ammonium oxide and anhydrous sodium sulfate, extract homogeneously, centrifuge, transfer the supernatant to a chicken heart bottle; concentrate the supernatant in the chicken heart bottle to dryness; dissolve with water, sonicate, add n-hexane, vortex and mix, and let stand to separate layers. , discard the n-hexane in the upper layer, add n-hexane and vortex to mix, let it stand for layering, transfer the water phase to a centrifuge tube, centrifuge, filter the membrane, and use it for high-performance liquid chromatography-tandem mass spectrometry measurement; in addition, accurately weigh the chlorine The mycin standard is dissolved and fixed to volume with chromatographic methanol and ultrasonic, and is prepared into solutions of different concentrations; measured by high-performance liquid chromatography-tandem mass spectrometry; a standard curve is obtained; the obtained test data is calculated through the standard curve to calculate the concentration of chloramphenicol in the sample to be tested ; The method of the present invention has good accuracy, high precision and good linearity.
CN201610180245 discloses a HPLC method for simultaneously determining the residual amounts of trinexapac-ethyl and trinexapac-ethyl in wheat. After the wheat sample is prepared, it is extracted with acetonitrile vibration, filtered and concentrated to nearly dryness, and then diluted to volume with methanol through acid chromatography. , after adding silica gel and anhydrous magnesium sulfate for dispersive solid phase extraction and purification, vortex, centrifuge, and pass through a microporous membrane to form a sample solution; the sample solution was measured using a high-performance liquid chromatograph with a UV detector, and the chromatographic column was Agilent- Zorbax chromatographic column, column temperature is 35°C, flow rate is 0.6mL/min, injection volume is 20uL, mobile phase is a mixed solution composed of methanol and 0.1% phosphoric acid aqueous solution with a mass concentration of 0.1%. The volume ratio of methanol and phosphoric acid aqueous solution is 65: 35, the wavelength is 280nm, and the external standard method is used to quantitatively determine the content of trinexapac-ethyl and trinexapac-ethyl.
CN201811249677 discloses a method for extracting, purifying and testing astragaloside from Astragalus chinensis, which relates to the field of extraction, purification and testing of active substances from Astragalus chinensis. It uses 70% ethanol as the extractant and uses a microwave-ultrasonic assisted extraction instrument. After auxiliary treatment, the crude extract of astragaloside was obtained. Using a mixed solution of chloroform, methanol, ethyl acetate, and water as the developing agent, the crude extract was prepared through thin film.Chromatographic development is used to separate and purify astragaloside IV and astragalus saponins I, II, and III, using chromatographic methanol and ultrapure water as the mobile phase, and using a high-resolution mass spectrometer to accurately measure the molecular mass information of the sample (the mass charge of the molecular ion or fragment ion ratio), its functional groups were detected by infrared, and its molecular structure was analyzed. Finally, its optical rotation, specific optical rotation and melting point were measured. The application of TLC-MS-IR tandem technology to detect astragaloside in astragalus mushrooms can realize separation and preparation from microgram level to gram level. It is a simple, short and efficient extraction, purification and detection method. Methods.
Main reference materials
[1]CN201510000448.8 A method for isolation and purification of tartirelin
[2]CN201710159438.8 Quantitative detection method of abiraterone in whole blood
[3]CN201110429196.2 HPLC-MS-MS detection method for chloramphenicol residues in functional foods
[4]CN201610180245.6 A HPLC method for simultaneous determination of trinexapac-ethyl and trinexapac-ethyl residues in wheat
[5]CN201811249677.3 A method for extraction, purification and detection of astragaloside from Astragalus chinensis
