31 results about "Impurity profiling" patented technology

The invention relates to a 5,6,4'-trihydroxyl flavone-7-O-D-glucuronic acid related substance b which is successfully prepared through selective elimination and hydrolysis by taking 5,6,4'-triacetoxy flavone-7-O-D-triacetyl methyl glucuronate (the structural formula is as shown in a formula II) as a raw material. The related substance b is further purified, and finally, a 5,6,4'-trihydroxyl flavone-7-O-D-glucuronic acid related substance b monomer is obtained to obtain a related substance chemical structure after confirmation. The method is short in synthetic route, low in cost, simple to operate, accurate in result, high in product purity, high in reaction yield and easy for product purification, and can be used for impurity analysis and control of a synthesized 5,6,4'-trihydroxyl flavone-7-O-D-glucuronic acid sample, so that quality control of the synthesized 5,6,4'-trihydroxyl flavone-7-O-D-glucuronic acid is facilitated, and the product quality is better guaranteed.

The invention relates to an impurity analysis method for multiple vitamin preparations. The method comprises the following steps of preparing a test solution of the vitamin preparations; dissolving o-phthalaldehyde and 2-mercaptoethanol based on a mass ratio of 1 to (2-5) in methanol, adding a boric acid buffer solution, and adjusting the pH value to 3-5 to obtain a derivatization reagent; and taking the test solution, adding the derivatization reagent to carry out online derivatization reaction, and injecting the derivatized test solution into a high performance liquid chromatograph, therebydetecting impurities in the test solution. According to the method, folic acid impurity A, folic acid impurity D, p-aminobenzoic acid and 3-aminopropanol in the vitamin preparations can be effectivelydetected; and the method is high in sensitivity and good in specificity.

The invention relates to the field of high-purity gas impurity detection and specifically relates to a method for increasing detection sensitivity of special impurities in high-purity hydrogen chloride. According to the method for increasing detection sensitivity of special impurities in high-purity hydrogen chloride disclosed by the invention, two parallel chromatographic columns are used; an independent temperature-control column box is adopted, so that column temperatures of the two parallel chromatographic columns can be guaranteed, and such an arrangement is beneficial to respectively separated components; a helium ion detector is used for detecting trace impurities and the limit of detection can be reduced to 1-10ppb; a filler special for high-purity hydrogen chloride chromatographicanalysis and nanometer titanium dioxide are adopted for modifying a capillary column, so that the separation of trace impurities in electronic hydrogen chloride can be boosted; the helium ion detector is used for detecting hydrogen chloride according to the method, so that the sensitivity is high and the limit of detection is low; impurity component response is linear; after a gas flow is designed, sample can be injected at one time and the requirements for analyzing all the impurities of electronic hydrogen chloride gas can be met.

The invention discloses an impurity HPLC analysis method for nedaplatin. In the method, octadecylsilane bonded silica gel is used as a filler (recommendation: AQ-C18), the detection wavelength is 205-222nm, and the column temperature is 20~45℃, the mobile phase is a mixture of pH6.0~8.5 buffer and polar organic solvent, characterized in that the mobile phase is to elute the impurities in the nedaplatin sample by gradient elution, pH6. The initial ratio of 0-8.5 buffer solution to polar organic solvent is 100:0-90:10, and the final ratio is 90:10-60:40; the flow rate of mobile phase is 0.5-1.0ml / min; prepared with mobile phase into a solution containing 0.5 mg to 2 mg / ml of nedaplatin; inject 5 μl to 20 μl of the sample solution into a high performance liquid chromatograph, record the chromatogram and perform sample analysis. After using the HPLC analysis method of the present invention, the theoretical plate number of the main peak of the product is obviously increased, and more impurities can be separated, so that the accuracy of analyzing the nedaplatin sample is improved.

The invention belongs to the field of synthesis of medicines, and specifically relates to a preparation method for a sarpogrelate hydrochloride photodegradable impurity III. The sarpogrelate hydrochloride photodegradable impurity III is prepared by comprising five-step reactions of substitution reaction, addition reaction, esterification reaction, epoxidation reaction and reduction reaction with 2-[2-(3-methoxyphenyl)vinyl]phenol as a raw material; and after column chromatography separation of a crude sarpogrelate hydrochloride photodegradable impurity III, purity reaches more than 99%. The preparation method provided by the invention has simple operation and mild reaction; the sarpogrelate hydrochloride photodegradable impurity III has high purity and can be applied in analysis of impurity profiling; and total yield is high.

The invention discloses an ultra-high performance liquid chromatography analysis method for dihydralazine sulfate and its related substances. Waters UPLC AcQuity H-Class is used, a reversed-phase C18 column is used, and potassium dihydrogen phosphate-phosphate buffer is used as the mobile phase A, Gradient elution with methanol as mobile phase B. The method can effectively control the known impurity content through the principal component self-contrast method with a correction factor, and the separation between the main peak and adjacent impurity peaks and between each impurity peak is greater than 1.5. The method of the application is simple, easy to operate, and has good reproducibility, accurate analysis and positioning of impurities, and can provide a reliable analysis method for controlling the quality of dihydralazine sulfate and its tablets.