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Method for detecting related substances in chloral hydrate

A chloral hydrate and detection method technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems that chloral hydrate raw materials and related preparations have not been found, and achieve clinical efficacy, good stability and repeatability, and sensitivity high effect

Active Publication Date: 2019-03-01
SHANDONG DYNE MARINE BIOTECHCAL PHARM HLDG CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

After searching domestic and foreign literature and patents, no report has been found on the inspection method of related substances in chloral hydrate raw materials and related preparations

Method used

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  • Method for detecting related substances in chloral hydrate
  • Method for detecting related substances in chloral hydrate
  • Method for detecting related substances in chloral hydrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] Embodiment 1, determination of related substances of chloral hydrate suppository

[0069] The instrument uses Agilent 7890B gas chromatograph + Agilent 5977B mass spectrometer detector; METTLER XP205 electronic balance.

[0070] The material is the chloral hydrate suppository prepared by the technology center of our company and the chloral hydrate suppository of Japan Hisamitsu Pharmaceutical;

[0071] The formic acid reference substance was purchased from Anaqua Chemicals Supply, the batch number was 73C1512FE; the chloroform reference substance was purchased from Anaqua Chemicals Supply, the batch number was 38Y1504MA; the trichloroethanol reference substance was purchased from Aladdin, the batch number was C1512073; the dichloroacetic acid reference substance was purchased from Aladdin, The batch number is K1715066; the trichloroacetic acid reference substance was purchased from Aladdin, the batch number is K1713111;

[0072] Ethanol and n-heptane are chromatographi...

Embodiment 2

[0122] Embodiment 2, linearity test

[0123] 1. Prepare a series of impurity reference substance solutions with different concentrations

[0124] Precisely measure 1, 2, 2, 4, 2, 6, 3ml of impurity reference substance stock solution (2.5mg / ml), respectively put them in 50, 50, 20, 25, 10, 25, 10ml measuring bottles, add ethanol Dilute to the mark and shake well to obtain the linear test solution for impurities of each concentration.

[0125] 2. Carry out GC-MS detection of each impurity reference substance solution, and the detection conditions are as follows:

[0126] Detection condition is all the same as embodiment 1

[0127] After the GC-MS detection is completed, record the peak area of ​​each impurity and each concentration of the reference substance, with the concentration as the independent variable and the corresponding peak area as the dependent variable, to obtain a linear regression equation:

[0128] The obtained results are shown in Tables 6-10;

[0129] Tabl...

Embodiment 3

[0144] Embodiment 3, specificity test

[0145] 1. Preparation of the test solution

[0146] With embodiment 1;

[0147] 2. Preparation of each impurity reference substance solution

[0148] With embodiment 1;

[0149] 3. Preparation of negative control solution

[0150] Accurately weigh about 400 mg of the blank of the content of the chloral hydrate suppository, and put it in a 25 ml stoppered colorimetric tube, accurately add 2 ml of ethanol, 2 ml of 20% sulfuric acid ethanol solution (V / V), 0.1 g of anhydrous magnesium sulfate, and close the plug. Vortex to dissolve, heat in a water bath shaker at 50°C for 40 minutes, take it out and shower quickly, add 4ml of n-heptane precisely, vortex to mix, add 20ml of water, shake, stand to separate layers, take the supernatant as Negative control solution.

[0151] 4. Determination of impurity content in the test solution and negative control solution

[0152] Carry out GC-MS analysis to above-mentioned impurity reference substa...

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Abstract

The invention provides a method for detecting a chloral hydrate raw material and chloral hydrate suppository related substances. The method comprises the steps of carrying out derivatization reactionand then carrying out GC-MS detection. The method is good in specificity and high in sensitivity, the stability and repeatability of the method are good, the analyzing efficiency is high, various impurities of chloral hydrate suppository can be qualified and quantified sensitively and accurately, therefore, the quality of the chloral hydrate suppository is evaluated objectively, comprehensively and accurately, and the method plays an important significance on control over the quality of the chloral hydrate suppository and guaranteeing the clinical effects.

Description

technical field [0001] The method belongs to the technical field of drug analysis, and relates to a method for detecting related substances of chloral hydrate raw material and chloral hydrate suppository. Background technique [0002] Chloral hydrate is a short-acting sedative drug, commonly used in pediatric clinics, with quick onset of administration, high safety, similar to physiological sleep, the therapeutic dose does not inhibit breathing, no obvious side effects, and good compliance. At present, there are no related substance inspection items in the quality standards of chloral hydrate raw materials and related preparations (chloral hydrate-free suppository type) recorded in the US Pharmacopoeia, British Pharmacopoeia, European Pharmacopoeia, Japanese Pharmacopoeia and Chinese Pharmacopoeia. According to domestic and foreign literature and patent searches, no reports on related substance inspection methods for chloral hydrate raw materials and related preparations hav...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 李洪卫何淑旺景亚军胡醒王建村陶元景
Owner SHANDONG DYNE MARINE BIOTECHCAL PHARM HLDG CO LTD
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