Method for determining content of 4-cyanopyridine and impurities of 4-cyanopyridine in isoniazide starting material
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A kind of technology of cyanopyridine, determination method, applied in the field of analytical chemistry
Inactive Publication Date: 2018-06-29
CHONGQING HUABANGSHENGKAI PHARM
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[0005] Among the detection methods currently reviewed, there is no pharmacopoeia or literature report that a detection method can simultaneously separate and detect multiple impurities of the key starting material SM1
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Embodiment 1
[0099] Embodiment 1 Determination of related substances of 4-cyanopyridine SM1
[0100] 1. Instruments and conditions
[0101] Table 1 Instrument and chromatographic conditions
[0102]
[0103]
[0104] 2. Experimental steps
[0105] (1) Take an appropriate amount of impurity SM1a, impurity SM1c, impurity SM1d, impurity SM1e and this product, add methanol to dissolve and dilute to make about 0.01mg of impurity SM1a, impurity SM1c, impurity SM1d, impurity SM1e and SM1 10mg per 1ml solution, as a system suitability solution.
[0106] (2) Take this product, weigh it accurately, add methanol to dissolve and dilute to make a solution containing about 10 mg per 1 ml, as the test solution.
[0107] (3) Accurately measure 1ml of the test solution, put it in a 100ml measuring bottle, dilute to the mark with methanol, shake well, and use it as a control solution.
[0108] (4) Weigh an appropriate amount of each impurity reference substance and the test sample, add diluent met...
Embodiment 2
[0121] Embodiment 2 Several batches of 4-cyanopyridine related substance assay results
[0122] According to the method of Example 1, several batches of 4-cyanopyridine samples from our company were tested for related substances. The calculation results are shown in Table 3.
[0123] Table 3 Test results of several batches of samples
[0124]
[0125] The method provided by the invention only uses gas chromatography to separate and measure 4-cyanopyridine and its related substances, and can effectively separate other solvent peaks so that it does not interfere with the detection of related substances. The method has the advantages of good separation, strong specificity, high sensitivity, and simple operation, and has the advantages of simplicity and speed.
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Abstract
The invention belongs to the field of analytical chemistry, and particularly relates to a method for determining the content of 4-cyanopyridine and impurities of 4-cyanopyridine in an isoniazide starting material. The measuring method is a gas chromatographic method, and comprises the following specific steps: vaporizing a sample in a vaporization chamber, and introducing the vaporized sample intoa chromatographic column through flowing gas; separating the 4-cyanopyridine SM1 and the impurities of 4-cyanopyridine by means of programmed heating; calculating the content of the impurities by using a principal component self-contrasted method with a correction factor. At present, no reports of simultaneous separation and determination of a plurality of impurities in the SM1 exist. The methodfor measuring the content of the plurality of impurities in the SM1 provided by the invention is simple and feasible, and has high sensitivity and high specificity, so that established quality controlitems of SM1 relevant substances can improve the quality controllability and safety of a product when being applied to control of relevant substances of the product.
Description
technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for separating and measuring the content of isoniazid starting material 4-cyanopyridine and impurities by gas chromatography. Background technique [0002] Isoniazid is widely used as a first-line anti-tuberculosis drug, and its synthetic route is relatively simple. The synthesis of isoniazid in our company is the key starting material 4-cyanopyridine (SM1) in water with sodium hydroxide as a catalyst. The hydrolysis reaction gives the intermediate Z1; the substitution reaction between the intermediate Z1 and hydrazine hydrate in water gives the crude product Z of isoniazid; the crude product Z is refined in purified water to get the finished product of isoniazid. Concrete synthesis process route is as follows: [0003] [0004] In order to strictly control the quality of isoniazid, we plan to control the impurities from the source of the key starting ...
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