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Detection method for limit of sulfite

A technology of sulfite and detection method, which is applied in the preparation of test samples, material analysis by observing the influence on chemical indicators, and analysis by chemical reaction of materials, etc., to achieve low cost of reagents and equipment, reagents And the cost of equipment is safe, non-toxic, non-polluting, and easy to operate.

Active Publication Date: 2016-06-29
BEIJING VOBAN PHARMA TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Barium sulfite is slightly soluble in water, and its solubility in water at 25°C is 0.011mg / mL, and its ion product K sp About 5.3×10 -7 , and the solubility of barium sulfite is greater under acidic conditions. Therefore, the sulfate limit test method is not suitable for the sulfite limit test. How to quickly and accurately detect whether the residual amount of sulfite in the drug meets the requirements is an urgent need solved problem

Method used

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  • Detection method for limit of sulfite
  • Detection method for limit of sulfite
  • Detection method for limit of sulfite

Examples

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Embodiment 1

[0142] The inspection method of sulfite limit in embodiment 1 ofloxacin crude drug:

[0143] (1) Accurately weigh 196.9 mg of anhydrous sodium sulfite (equivalent to 100 mg of SO 2 ), put it in a 100ml measuring bottle, add purified water to dissolve and dilute to the scale, and shake up; accurately measure 1ml, put it in a 10ml measuring bottle, add purified water to dilute to the mark, shake up, and use it as a standard sodium sulfite solution (containing SO 2 The concentration is 100 μg / ml).

[0144] (2) Accurately weigh 1.0 g ofloxacin bulk drug, add 30 ml of water, shake fully to obtain a yellow transparent solution, put the filtrate in a 50 ml Nessler colorimetric tube, add 2 ml of dilute hydrochloric acid of 10% mass fraction, add 30 % hydrogen peroxide 2ml, shake well, that is the test solution. Prepare another test solution in the same way.

[0145] (3) Take a portion of the test solution, add 2ml of 30% hydrogen peroxide, add 5ml of 25% barium chloride solution, l...

Embodiment 2

[0148] Embodiment 2 The inspection method of the sulfite limit in the ezetimibe bulk drug comprises the following steps:

[0149] (1) Accurately weigh 196.9 mg of anhydrous sodium sulfite (equivalent to 100 mg of SO 2 ), put it in a 100ml measuring bottle, add purified water to dissolve and dilute to the scale, and shake up; accurately measure 1ml, put it in a 10ml measuring bottle, add purified water to dilute to the mark, shake up, and use it as a standard sodium sulfite solution (containing SO 2 The concentration is 100 μg / ml).

[0150] (2) Accurately weigh 1.0 g of ezetimibe crude drug, add appropriate amount of water, shake fully, filter, put the filtrate in a 50 ml Nessler colorimetric tube, add water to 40 ml, add 2 ml of dilute hydrochloric acid, add 3 ml of 20% hydrogen peroxide, Shake well to obtain the test solution.

[0151] (3) Take 1ml of standard sodium sulfite solution, put it in a 50ml Nessler colorimetric tube, add water to make about 40ml, add 2ml of dilut...

Embodiment 3

[0153] The inspection method of sulfite limit in the gelatin hollow capsule shell of embodiment 3 comprises the following steps:

[0154] (1) Accurately weigh 246.9 mg of anhydrous potassium sulfite (equivalent to 100 mg of SO 2 ), put it in a 100ml measuring bottle, add purified water to dissolve and dilute to the mark, and shake up; accurately measure 1ml, put it in a 10ml measuring bottle, add purified water to dilute to the mark, shake up, and use it as a standard potassium sulfite solution (containing SO 2 The concentration is 100 μg / ml).

[0155] (2) Accurately weigh 2.0g of gelatin hollow capsule shell, add appropriate amount of water, shake fully, filter, put the filtrate in a 50ml Nessler colorimetric tube, add water to make 40ml, add 2ml of dilute hydrochloric acid, add 2ml of 30% hydrogen peroxide, Shake well to obtain the test solution.

[0156] (3) Take 2ml of standard potassium sulfite solution, put it in a 50ml Nessler colorimetric tube, add water to make about ...

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Abstract

The invention provides a detection method for the limit of sulfite. The detection method includes the following steps that 1, a sulfite standard solution is prepared; 2, the value of the drug taking amount w is obtained through calculation; 3, a test product solution is prepared; 4, a contrast solution is prepared; 5, the test product solution and the contrast solution are arranged in a first colorimetric tube and a second colorimetric tube respectively; then an excessive barium chloride solution is added to the test product solution and the contrast solution respectively, water is used for volume fixing till the volume is V4, full shaking-up is conducted, and standing is conducted for 0-120 min; whether turbidity generated by the test product solution is lower than that generated by the contrast solution or not is observed through a visual observation method; if yes, the content of sulfite in a detected drug is lower than the value of the weight limit a, and the detected drug meets the requirement. The detection method has the advantages of detecting the limit of sulfite in the drug and being easy to operate, high in sensitivity, low in needed reagent and equipment cost, safe and free of toxins and pollution.

Description

technical field [0001] The invention belongs to the technical field of sulfite detection, and in particular relates to a detection method for sulfite limit. Background technique [0002] Sulfites include sodium sulfite, sodium bisulfite, potassium bisulfite, sodium hyposulfite, sodium pyrosulfite, potassium pyrosulfite, and the like. In the pharmaceutical preparation process, because sulfites are often used as raw materials or reducing agents, or when some easily degradable reagents (such as thionyl chloride) are used, sulfites will be generated after hydrolysis, so the final preparation Sulfite residues are often present in the obtained pharmaceutical products. [0003] Sulfite residues in medicines are harmful to the human body. For example, the patent CN104833639 describes feeding rats with feed containing 0.1% sodium sulfite for 2 years, and the development of the rats is inhibited; feeding rats with feed containing 0.1% sodium sulfite for 2 years, neuritis, bone marro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/82G01N1/28
CPCG01N1/28G01N21/82
Inventor 冯连松罗林张卫锋
Owner BEIJING VOBAN PHARMA TECH CO LTD