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Method for Determination of Soluble Mercury and Valence Mercury in Drugs Containing Cinnabar

A soluble and cinnabar technology, applied in the direction of measuring devices, preparation of test samples, and material analysis by electromagnetic means, can solve the problems of lack of scientific basis for usage and dosage, unknown material basis, and difficulty in rationally evaluating safe doses, etc., to achieve filling Domestic blank, sensitive effect of the method

Active Publication Date: 2017-05-17
SHANGHAI INST FOR FOOD & DRUG CONTROL
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the lack of scientific basis for usage and dosage, it is difficult to reasonably evaluate its safe dose, and the problem of drug safety has been plagued by my country's traditional Chinese medicine industry
[0004] 2. The unknown material basis of cinnabar efficacy and toxicity has seriously hindered its international recognition:
The current quality standards for cinnabar only control the total amount of mercury, but do not control the content of soluble mercury and valence mercury, which cannot reflect the actual application of cinnabar in the human body. It is unreasonable to measure whether it is safe or not by the total amount of elements. not scientific
[0006] 3. The existing quality standards of cinnabar cannot reflect the effectiveness and safety, and there is no basis for usage and dosage:
[0007] my country's 2010 edition of "Chinese Pharmacopoeia" under the cinnabar item only contains the redox titration method for content determination; it lacks scientific quality control methods for effective ingredients and limited control methods for toxic ingredients; and its usage and dosage lack scientific basis , it is urgent to further improve the
[0008] 4. A large number of cinnabar-containing preparations lack relevant research and quality control methods, leading to safety problems in practical applications:
Through literature review, it is found that the methods of soluble mercury in cinnabar reported in each literature are basically similar, using artificial gastric juice or artificial intestinal juice as the extraction solvent, but the obtained soluble mercury content is quite different

Method used

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  • Method for Determination of Soluble Mercury and Valence Mercury in Drugs Containing Cinnabar
  • Method for Determination of Soluble Mercury and Valence Mercury in Drugs Containing Cinnabar
  • Method for Determination of Soluble Mercury and Valence Mercury in Drugs Containing Cinnabar

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Determination of soluble mercury content in cinnabar medicinal materials: according to inductively coupled plasma mass spectrometry (Appendix XI D of Chinese Pharmacopoeia 2010 edition).

[0063] Reagents and Instruments

[0064] 7700ce inductively coupled plasma mass spectrometer from Agilent, USA; B9500S-DTH ultrasonic cleaner (power 300W, frequency 45kHz) from Branson Ultrasound (Shanghai) Co., Ltd.; Milli-Q ultrapure water machine from Millipore, USA. Mercury standard solution (1000 mg / L, batch number HC931554), purchased from Merk Company.

[0065] Nitric acid and hydrochloric acid were both excellent grade pure (Merck company); pepsin was a biochemical reagent, the enzyme activity was 1:27000, and the batch number was 100710, purchased from Shanghai Huixing Biochemical Reagent Co., Ltd.; trypsin was a biochemical reagent, casein converting capacity ≥25.0, the batch number is F20100714, purchased from Sinopharm Chemical Reagent Co., Ltd.; the water is deionized wa...

Embodiment 2

[0110] Determination of soluble mercury content in cinnabar decoction pieces: according to inductively coupled plasma mass spectrometry (Appendix XI D of Chinese Pharmacopoeia 2010 edition).

[0111] The cinnabar medicinal material in Example 1 was replaced with cinnabar decoction pieces (derived from Guizhou Tongren Mining Industry, processed by Shanghai Fengbang Traditional Chinese Medicine Piece Factory, batch number H2008030502), and other methods and processes were the same as in Example 1.

[0112] Solution stability test:

[0113] Get the cinnabar decoction pieces, prepare the test solution according to the same method of preparing the test solution in Example 1 "Determination of the content of soluble mercury in the medicinal material of cinnabar", and analyze the samples at different times to measure the amount of soluble mercury, the results show (see table 4), the soluble mercury content in the test solution is basically stable within 0 to 24 hours.

[0114] Table ...

Embodiment 3

[0151] Determination of soluble mercury content in cinnabar preparations: according to inductively coupled plasma mass spectrometry (Appendix XI D of Chinese Pharmacopoeia 2010 edition).

[0152] Preparation of the test solution: take Jufang Zhibao Powder (provided by Wuhan Jianmin Dapeng Pharmaceutical Co., Ltd., batch No. 4) 150mg, grind finely, accurately weigh, (1) put a 250ml glass measuring bottle (first use 20% hydrochloric acid) The solution (v / v) was soaked overnight, then washed with deionized water and air-dried), added artificial intestinal juice to the volume, shaken well, tightly plugged, weighed, and placed at 37°C for ultrasonic treatment (power 300W, Frequency 45kHz) for 2 hours, shake once every 10-15 minutes, or (2) put a 250ml ~ 500ml conical flask with stopper (soak in 20% hydrochloric acid solution (v / v) overnight, then use deionized water Wash and dry), add 250ml of artificial intestinal juice, shake well, weigh the fixed weight, place it in a 37°C water...

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Abstract

The invention discloses a method for determining the content of soluble mercury in cinnabar-containing drugs, characterized in the following steps: (1) that the soluble mercury is extracted from the cinnabar-containing drugs by an ultrasonic treatment and / or a magnetic stir with a bionic solvent; (2) that preferably a solution extracted in step (1) is purified; and (3) that an ICP-MS method is used to determine the content of the soluble mercury in the cinnabar-containing drugs. The invention also discloses a method for determining the content of soluble valence-state mercury in the cinnabar-containing drugs. In the invention the method for determining cinnabar drug effects and main toxicity components is established by simulating extraction manners in bodies and by adopting the ICP-MS method and an HPLC-ICP-MS method. In addition, the method is sensitive and accurate.

Description

technical field [0001] The invention relates to a method for determining the content of soluble mercury in medicines containing cinnabar by using a biomimetic extraction-ICP-MS method, and also relates to a method for determining the soluble valence state in medicines containing cinnabar by using a biomimetic extraction-HPLC-ICP-MS method method for mercury content. Background technique [0002] Cinnabar is a commonly used mineral traditional Chinese medicine in my country. It has been used clinically for thousands of years. The earliest recorded medicine is "Shen Nong's Materia Medica". It can be taken internally and externally and has a wide range of uses. Traditional medicine believes that cinnabar has the functions of clearing the heart and calming anxiety, soothing the nerves and detoxifying, and is listed as the first sedative and tranquilizing medicine by some Chinese medicine. Since the 1950s, the sedative and tranquilizing effect of cinnabar has been confirmed by m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/64G01N1/34G01N30/72G01N30/02G01N30/08
Inventor 夏晶胡青季申王柯李丽敏王欣美张甦王枚博毛秀红郑荣吴赵云郏征伟苗水陆继伟陈铭于建简龙海钟吉强孙健孟茜毛丹许勇王少敏张道广陈静
Owner SHANGHAI INST FOR FOOD & DRUG CONTROL
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