Method for determining content of sulfite in medicinal materials by headspace gas chromatography-mass spectrometry

A headspace gas chromatography and sulfite technology, which is applied in the field of detection of sulfite content in medicinal materials, can solve the problems of inaccurate detection results, prolonged reaction time, and high temperature of the headspace bottle, so as to overcome the reaction time and equilibrium time. Shortened, high-accuracy effects

Active Publication Date: 2014-12-24
GANSU CHEEZHENG TIBETAN MEDICINE CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is that in the detection method of measuring sulfite in medicinal materials by headspace sampling method in the prior art, the detection result is inaccurate when the temperature of the headspace bottle is high, and the problem that the reaction time is prolonged when the temperature of the headspace bottle is low, Furthermore, by selecting an appropriate method and reasonable parameter settings, the contradiction between the reaction time and reaction temperature of the sample pretreatment is overcome, and a fast headspace gas chromatography-mass spectrometry with high accuracy, good repeatability, and short detection time is provided. Method for detecting sulfite content in medicinal materials

Method used

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  • Method for determining content of sulfite in medicinal materials by headspace gas chromatography-mass spectrometry
  • Method for determining content of sulfite in medicinal materials by headspace gas chromatography-mass spectrometry
  • Method for determining content of sulfite in medicinal materials by headspace gas chromatography-mass spectrometry

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Experimental program
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Effect test

Embodiment 1

[0035] (1) Accurately weigh 0.50 g of sodium sulfite solid powder, add it into a 100ml volumetric flask for ultrasonic dissolution, and constant volume to obtain a standard stock solution; respectively take 100, 200, 400, 800, 1600 and 3200 μl of the standard stock solution, Dilute to 25 ml volumetric flasks numbered A1, A2, A3, A4, A5 and A6 in turn to obtain 20, 40, 80, 160, 320 and 640 μg / ml sodium sulfite standard solutions;

[0036] (2) Add 2 g of pulverized Lycium sulfite-free granules, 400 μl of 20 μg / ml sodium sulfite standard solution to the headspace vial numbered B1, and then add 5 ml of 10 % sulfuric acid solution, quickly seal the bottle cap, shake up to obtain the standard test solution C1, the sulfite content of the unit medicinal material in the standard test solution C1 is 5 ppm after conversion;

[0037] According to the method of step (2), add 2 g of pulverized Lycium barbarum granules without sulfite to the headspace vials numbered B2, B3, B4, B5, and B6, a...

Embodiment 2

[0042] (1) Accurately weigh 0.50 g of sodium sulfite solid powder, add it into a 100ml volumetric flask for ultrasonic dissolution, and constant volume to obtain a standard stock solution; respectively take 100, 200, 400, 800, 1600 and 3200 μl of the standard stock solution, Dilute to 25 ml volumetric flasks numbered A1, A2, A3, A4, A5 and A6 in turn to obtain 20, 40, 80, 160, 320 and 640 μg / ml sodium sulfite standard solutions;

[0043] (2) Add 2 g of pulverized sulfite-free angelica granules, 400 μl of 20 μg / ml sodium sulfite standard solution, and then add 5 ml of 25% sulfuric acid solution, quickly seal the bottle cap, shake well to obtain the standard test solution C1, the sulfite content of the unit medicinal material in the standard test solution C1 is 5 ppm after conversion;

[0044] According to the method of step (2), add 2 g of crushed sulfite-free Angelica granules into the headspace vials numbered B2, B3, B4, B5, and B6 respectively, and add them to different head...

Embodiment 3

[0049] (1) Accurately weigh 0.50 g of sodium sulfite solid powder, add it into a 100ml volumetric flask for ultrasonic dissolution, and constant volume to obtain a standard stock solution; respectively take 100, 200, 400, 800, 1600 and 3200 μl of the standard stock solution, Dilute to 25 ml volumetric flasks numbered A1, A2, A3, A4, A5 and A6 in turn to obtain standard solutions of 20, 40, 80, 160, 320 and 640 μg / ml;

[0050] (2) Add 2 g of pulverized sulfite-free Codonopsis granules to the headspace vials numbered B1, B2, B3, B4, B5, and B6, and add them to different headspace vials in turn. 400 μl of sodium sulfite standard solutions with concentrations of 20, 40, 80, 160, 320 and 640 μg / ml respectively, and finally add 8 ml of sulfuric acid solution with a mass concentration of 30% to different numbered headspace vials, and quickly seal the vials Cover, shake well, and obtain standard test solutions C1, C2, C3, C4, C5, and C6 in sequence. After conversion, the sulfite conte...

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Abstract

The invention discloses a method for determining content of sulphur dioxide in medicinal materials by headspace gas chromatography-mass spectrometry, wherein a proper method is chosen and a reasonable parameter adjustment is performed, the temperature of a headspace bottle is set to be 45-55 DEG C, and the balance time is set to be 5-10 minutes; and preferably, the temperature of the headspace bottle is set to be 50 DEG C, and the balance time is set to be 5 minutes, so that the detection time for a single sample is obviously shortened, and the technical prejudice of prolonging the reaction time and / or increasing the reaction temperature to ensure the adequate release of sulphur dioxide in the prior art is solved. Compared with the measured result of a pharmacopoeia method, the method is high in accuracy and good in repeatability.

Description

technical field [0001] The invention relates to a method for detecting sulfite content in medicinal materials, in particular to a method for rapidly detecting the content of sulfite in medicinal materials by gas chromatography-mass spectrometry. Background technique [0002] It is common for some Chinese medicinal materials, fruits and vegetables, edible fungi, etc. to be smoked with sulfur. During the process of sulfur fumigation, as the temperature rises, the moisture, salt and SO 2 The reaction formed sulfites, which remained on the surface. Excessive consumption of sulfite can stimulate the bronchi and lungs, which may induce various respiratory inflammations. Asthma patients are particularly sensitive to sulfur dioxide, and eating it will aggravate the condition and even cause death. Organs produce toxic effects. Therefore, the State Food and Drug Administration regulates SO in food and medicinal materials. 2 There are certain limit standards for residues. This requ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06
Inventor 王维波刘鸿雁
Owner GANSU CHEEZHENG TIBETAN MEDICINE CO LTD
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