Method for determining residual quantity of sulfur dioxide in Chinese herbal medicines

A technology of sulfur dioxide and Chinese medicinal materials, which is applied in the field of determination of residual sulfur dioxide in Chinese medicinal materials, and achieves the effects of low detection cost, safe operation and simple reaction method

Inactive Publication Date: 2014-01-22
成都捷洱健康科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there is no use of fluorescence derivatization method for the determination of sulfur dioxide residues in Chinese herbal medicines

Method used

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  • Method for determining residual quantity of sulfur dioxide in Chinese herbal medicines
  • Method for determining residual quantity of sulfur dioxide in Chinese herbal medicines
  • Method for determining residual quantity of sulfur dioxide in Chinese herbal medicines

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1 The present invention establishes the rapid detection method of sulfur dioxide in Chinese medicinal materials

[0042] (1) Take 1g of the fine powder of the Chinese herbal medicine to be tested, add 25mL of 0.5% w / v sodium hydroxide solution, at 40°C, 200r min -1 Shake and extract for 30min, filter, take 1.0mL filtrate and dilute to 25mL to obtain the test solution;

[0043] (2) Take sulfite as the reference substance, and prepare concentrations of 1, 3, 7, 12, 15, 18×10 -3 mmol·L -1 The reference substance solution;

[0044] (3) Take an appropriate amount of the test solution and the reference solution in a 10ml volumetric flask, first add 2.0mL of Na with pH=6.44 2 HPO 4 -KH 2 PO 4 buffer solution, then add 2.5mL1mmoL·L -1 Phthalaldehyde solution and 1.5mL5mmoL·L -1 Ammonium acetate solution, mix well, dilute with water, keep the temperature in a water bath at 50°C for 5 minutes, take it out, immediately put it in ice water to cool, stop the react...

Embodiment 2

[0045] Embodiment 2 The optimization of detection method of the present invention

[0046] (1) Condition screening of fluorescence derivatization reaction method

[0047] 1 Experimental part

[0048] 1.1 Instrument

[0049] RF-5301 (PC) S fluorescence spectrophotometer (Shimadzu Corporation of Japan); electronic analytical balance BP211D (1 / 100,000, German Sartorius Company), electronic analytical balance BP121S (1 / 10,000, German Sartorius Company); pHS- 3C acidity meter (Shanghai Leici Instrument Factory); WHY-2 water bath constant temperature oscillator (Jincheng Guosheng Experimental Instrument Factory, Jintan City, Jiangsu); constant temperature water bath W201B (Beijing Guohua Medical Instrument Factory).

[0050] 1.2 Reagents

[0051]Sodium sulfite (Chengdu Kelong Chemical Reagent Factory, batch number: 20110906, purity ≥ 97%); o-phthalaldehyde (Japan TCI company, batch number: 120324, purity ≥ 98%); other reagents were analytically pure, and the experimental water wa...

Embodiment 3

[0088] Embodiment 3 methodological investigation

[0089] 1 Preparation of the test solution

[0090] Take about 1 g of yam fine powder, weigh it accurately, add 25 mL of 0.5% sodium hydroxide solution accurately, shake well, shake and extract (200r min -1 , 40°C) for 30min, filter, and dilute 1.0mL to 25mL.

[0091] 2 linear relationship test

[0092]Precisely draw 0.1, 0.3, 0.7, 1.2, 1.5 and 1.8mL of sodium sulfite stock solution and dilute to 100mL with water, and then pipette 1.0mL of the above-mentioned dilutions of different concentrations, and measure the relative fluorescence intensity of the product according to the experimental method. Taking the fluorescence intensity as the ordinate, Na 2 SO 3 The addition amount of the reference substance (nmoL) is the abscissa, and the standard curve is drawn, and the regression equation is: Y=46.247X-15.007, r 2 =0.9998, indicating that Na 2 SO 3 The linear relationship is good within the range of 0.9997-17.99nmoL.

[00...

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Abstract

The invention provides a method for determining the residual quantity of sulfur dioxide in Chinese herbal medicines. The method comprises the following operation steps: (1) taking the Chinese herbal medicines to be determined, and preparing a test solution; (2) taking sulfite as a reference substance, and preparing a reference substance solution; (3) respectively taking the test solution and the reference substance solution, adding an ortho-phthalaldehyde solution and an ammonium salt solution for reaction in a buffer solution, standing after the reaction is over and stopped, and determining the residual quantity of sulfur dioxide in Chinese herbal medicines by a fluorescence derivatization method. According to the method for determining the residual quantity of sulfur dioxide in Chinese herbal medicines, the residual quantity of sulfur dioxide in Chinese herbal medicines can be accurately and fast determined, and the reaction method is simpler and more convenient and is higher in practicability while the accuracy is equivalent to that of a pharmacopoeia method.

Description

technical field [0001] The invention relates to a method for measuring residual sulfur dioxide in Chinese medicinal materials. Background technique [0002] Sulfur is an ancient drug used to prevent insects in traditional Chinese medicine. Many traditional Chinese medicinal materials are sulfur-fumigated when they are processed. There are many changes in the chemical composition, and the residual sulfur dioxide in the fumigated Chinese medicinal materials is very harmful to the human body. The 2005 edition of the "Chinese Pharmacopoeia" canceled the "sulfur fumigation curing method" for medicinal materials, and listed it in the appendix of the 2010 edition of the "Chinese Pharmacopoeia". Added the determination method of residual sulfur dioxide based on the distillation method. Since this method requires a special all-glass distillation instrument, its popularization is very slow. Chromatography and ion chromatography, etc., but the pararosaniline hydrochloride method needs...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/64G01N1/28
Inventor 刘友平陈鸿平彭月陈林银玲韦正樊丹青刘荣
Owner 成都捷洱健康科技有限公司
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