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Gas chromatography method of metoclopramide

A gas chromatographic analysis and metoclopramide technology, which is applied in the directions of analyzing materials, material separation, measuring devices, etc., can solve the problem of inability to comprehensively and accurately control the quality of metoclopramide preparations, unsatisfactory test results, and linearity. narrow range and other problems, to achieve the effect of low detection limit, simple method, good reproducibility and stability

Inactive Publication Date: 2016-04-13
JILIN NORMAL UNIV
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Problems solved by technology

However, the above-mentioned detection results are not ideal, and the quality of the metoclopramide preparation cannot be fully and accurately controlled.
For the above gas chromatography analysis method, the linear range: 0.30~30.00μg / ml, the linear range is narrow; the minimum detection concentration: 0.20μg / ml, the detection limit is low

Method used

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  • Gas chromatography method of metoclopramide
  • Gas chromatography method of metoclopramide
  • Gas chromatography method of metoclopramide

Examples

Experimental program
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Embodiment 1

[0036] (1) Preparation of reference substance solution

[0037] Accurately weigh 5.00 mg of the metoclopramide reference substance, put it in a 100ml volumetric flask, add absolute ethanol solution, dilute to the mark, and prepare a reference substance solution with a concentration of 50 μg / ml for future use.

[0038] (2) preparation of content determination need testing solution

[0039] Get 20 pieces of metoclopramide tablets, accurately weigh, grind finely, accurately take by weighing the sample fine powder of 1 / 20 of the total weight (approximately equivalent to 5 mg of metoclopramide), put in a 100ml volumetric flask, add Absolute ethanol solution, shake to dissolve, add absolute ethanol to dilute to the mark, shake well, filter with 0.45μm filter membrane, obtain the required test solution for content determination, set aside.

[0040] (3) Preparation of content uniformity determination need testing solution

[0041] Take 10 pieces of metoclopramide tablets, put them i...

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Abstract

The invention relates to a gas chromatography method of metoclopramide. The gas chromatography method comprises the following steps: (1) preparing a reference solution; (2) preparing a content determination test solution; (3) preparing a content uniformity determination test solution; (4) setting the following chromatographic conditions: a DB-5 capillary-column chromatography, nitrogen as a carrier gas, injection port at 300 DEG C, column oven at 280 DEG C, detector at 300 DEG C, carrier gas flow velocity of 1.0 ml / min, pad sweeping quantity of 3 ml / min, tail-blowing of 35 ml / min, split ratio of 30:1, sample size of 1 [mu]l, and adoption of a [mu]ECD detector; (5) testing in the way that 1 [mu]l of the reference solution and 1 [mu]l of the test solution are respectively precisely sucked and injected into a gas chromatograph for testing, the chromatogram for 10 min is recorded and peak area calculation is performed by the external standard method. The gas chromatography method of metoclopramide is simple and accurate, good in repeatability and stability, low in detection limit, quick in detection result analysis, and high in detection sensitivity, the numbers of theoretical plates all exceed 30,000, and the quality of metoclopramide can be controlled more comprehensively and effectively.

Description

technical field [0001] The invention relates to the field of chemical drug quality detection, in particular to a gas chromatography analysis method for chemical drug metoclopramide. Background technique [0002] Metoclopramide (N-[(2-diethylamino)ethyl]-4-amino-2-methoxy-5-chloro-benzamide), the molecular formula is C 14 h 22 ClN 3 o 2 , the molecular weight is 299.80. It is a commonly used antiemetic drug, which can be used for vomiting caused by brain tumor surgery, tumor radiotherapy and chemotherapy, sequelae of traumatic brain injury, acute craniocerebral injury and drugs. It also has a good effect on flatulence indigestion, loss of appetite, belching, nausea and vomiting. It can also be used for vomiting and motion sickness (ship) caused by sea and air operations. It can also reduce the nausea and vomiting reaction during barium meal examination, and promote the passage of barium; taking it before duodenal intubation is helpful for smooth intubation. It is somet...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/14
CPCG01N30/02G01N30/06G01N30/14G01N2030/025G01N2030/146
Inventor 孙艳涛赵磊乔春玉牡丹赵国升
Owner JILIN NORMAL UNIV
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