Method for determining content of 3-aminothiophene in bulk drug
An aminothiophene and bulk drug technology is applied in the field of determining the content of 3-aminothiophene in bulk drugs, and achieves the effects of short chromatographic time, high sensitivity and high polarity
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Embodiment 1
[0023] A method for measuring the content of 3-aminothiophene in a crude drug, comprising the steps of:
[0024] S1, get 3-aminothiophene reference substance, take the acetonitrile-1% formic acid aqueous solution that volume ratio is 1:9 as solvent, prepare the 3-aminothiophene solution of appropriate concentration, as reference substance solution; Get crude drug, take volume ratio as The acetonitrile-1% formic acid aqueous solution of 1:9 is solvent, prepares need testing solution;
[0025] S2, two parts of 3-aminothiophene reference substance solutions were prepared in parallel, and were detected by LC-MS / MS method to obtain the peak areas of 3-aminothiophene in the reference substance solution respectively;
[0026] S3, get the test solution and detect it by LC-MS / MS method to obtain the peak area of the test solution, and calculate the content of 3-aminothiophene in the test solution by the external standard method.
[0027] Specifically, the chromatographic conditions ...
Embodiment 2
[0033] The linear range investigation of the assay method that embodiment 1 provides
[0034] Accurately weigh 2.817mg of 3-aminothiophene oxalate into a 25mL volumetric flask, add acetonitrile to dissolve, dilute to the mark, shake well, and use it as 3-aminothiophene stock solution A; precisely pipette 1.8mL 3-aminothiophene stock solution Add solution A to a 20mL volumetric flask, add acetonitrile-1% formic acid aqueous solution with a volume ratio of 1:9 to dilute and constant volume, shake well, as 3-aminothiophene stock solution B; prepare 0.0507μg / mL, 0.1267μg / mL, 0.2535 μg / mL, 0.3042μg / mL, 0.3802μg / mL and 0.5069μg / mL linear solutions, labeled as L-LOQ, L-50%, L-100%, L-120%, L-150%, and L -200%.
[0035] According to the assay method provided in Example 1, sample injection was carried out successively, taking the peak area as the ordinate, and the concentration of the reference substance solution as the abscissa (μg / mL) to draw a standard curve, the results are shown ...
Embodiment 3
[0039] The sample addition recovery test of the assay method that embodiment 1 provides
[0040] Through the method of sample addition and recovery, the accuracy of the assay method provided in Implementation 1 was analyzed, and 62.5 mg of the raw material drug was taken, accurately weighed, placed in a 10mL volumetric flask, and 11 copies were parallelized, and 2 of them were taken to measure the 3-aminothiophene content; take 3 parts, add 0.25mL 3-aminothiophene stock solution B respectively, add acetonitrile-1% formic acid aqueous solution with a volume ratio of 1:9 to constant volume and mix, as 50% recovery rate of standard addition solution; get 3 parts thereof, add 0.5mL 3-aminothiophene stock solution B respectively, add acetonitrile-1% formic acid aqueous solution with a volume ratio of 1:9 to constant volume and mix, as 100% standard addition recovery solution; take which 3 parts, add 0.75mL 3-aminothiophene stock solution B respectively, add acetonitrile-1% formic a...
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