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Quick detection method of hydrocortisone

A hydrocortisone and detection method technology, applied in the field of analytical chemical detection, can solve the problems of insufficient fastness and flexibility, high cost, high detection requirements, etc., and achieve the effect of being conducive to observation, easy to operate, and obvious phenomena

Inactive Publication Date: 2017-06-09
SHANDONG INST FOR FOOD & DRUG CONTROL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention aims at the shortcomings of high detection requirements, high cost, and insufficient fastness and flexibility in the detection of hydrocortisone in the prior art, and provides a rapid detection method of hydrocortisone, which has the advantages of low analysis cost and no need for reference substances And relatively large analytical instruments, strong specificity, high sensitivity, high accuracy of test results, etc., suitable for on-site rapid detection of hydrocortisone added in Chinese patent medicines, health food and food

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1: the detection of tablet

[0028] Reagent preparation: extract is ethyl acetate; 1mol / L hydrochloric acid solution: take 9ml of hydrochloric acid, add appropriate amount of water to make 100ml, shake well; 1mol / L sodium hydroxide solution: take 4g of sodium hydroxide, add water 100ml, shake to dissolve ; Triphenyltetrazolium chloride test solution: take 0.5 g of triphenyltetrazolium chloride, add absolute ethanol to dissolve it to 100 ml.

[0029] Sample to be tested: Tongbi Tablet (produced by Yantai Bohai Pharmaceutical Group Co., Ltd., batch number: 131101, specification 0.3g, this product does not contain hydrocortisone as determined by LC-MS / MS method)

[0030] The detection method, the steps are: take 5 tablets, remove the colored coating, grind finely, take 0.5g, put it in a centrifuge tube with a stopper, add 5ml of 1mol / L hydrochloric acid solution, shake for 1min, add 5ml of ethyl acetate, shake vigorously Shake for 3 minutes, centrifuge to separ...

Embodiment 2

[0032] Embodiment 2: the detection of analog positive tablet sample

[0033] Reagent preparation: extract is ethyl acetate; 1mol / L hydrochloric acid solution: take 9ml of hydrochloric acid, add appropriate amount of water to make 100ml, shake well; 1mol / L sodium hydroxide solution: take 4g of sodium hydroxide, add water 100ml, shake to dissolve ; Triphenyltetrazolium chloride test solution: take 0.5 g of triphenyltetrazolium chloride, add absolute ethanol to dissolve it to 100 ml.

[0034] Sample to be tested: Tongbi Tablets (produced by Yantai Bohai Pharmaceutical Group Co., Ltd., batch number: 131101, specification 0.3g), take 5 tablets, remove the coloring coating, add 10 mg of hydrocortisone.

[0035] The detection method, the steps are: take 5 tablets, remove the colored coating, add 10 mg of hydrocortisone, grind finely, take 0.5 g, put it in a centrifuge tube with a stopper, add 5 ml of 1 mol / L hydrochloric acid solution, shake for 1 min, and then Add 5ml of ethyl acet...

Embodiment 3

[0037] Embodiment 3: the detection of syrup

[0038] Sample to be tested: Qiangli Pibalu (produced by Weifang Tianyang Pharmaceutical Co., Ltd., batch number: 160401, specification 180ml / bottle, this product does not contain hydrocortisone as determined by LC-MS / MS method)

[0039] The detection method, the steps are: take 3ml, put it in a centrifuge tube with stopper, add 5ml of 0.5mol / L hydrochloric acid solution, shake for 1min, add 5ml of ethyl acetate, shake vigorously for 3min, centrifuge to separate the layers, take the upper layer solution, Add an equal volume of 0.5mol / L sodium hydroxide solution, shake for 1min, centrifuge to separate layers, and the supernatant is used as the test solution; take 1 drop of 0.5mol / L sodium hydroxide solution, put it on a white porcelain drip plate, add Add 5 drops of triphenyltetrazolium chloride test solution, mix well, add 5 drops of the test solution, the color is negative (no red).

[0040] Result analysis: This product does not co...

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Abstract

The invention relates to the technical field of analytic chemistry detection, in particular to a quick detection method of hydrocortisone. The quick detection method includes: taking a to-be-detected sample, adding a hydrochloric solution, shaking, adding ethyl acetate, shaking, and centrifuging or standing for layering; taking centrifugate or upper-layer solution, adding a sodium hydroxide solution, shaking, and centrifuging or standing for layering; dripping the sodium hydroxide solution onto a white drip plate, dropwise adding a triphenyl tetrazolium chloride test solution, mixing well, dropwise adding a test sample solution, and observing color change. The quick detection method is simple and convenient to operate and low in analysis cost; interference of related factors is eliminated, and observation of solution color is facilitated better; extracting liquid, washing liquid, leaching liquid and a detection agent which are used in the method are high in specificity; interference substances are separated and removed by utilizing dissolubility difference of different substances for three times in the process of extracting, washing and leaching, so that sensitivity of chromogenic reaction is improved, detection result accuracy is high, the chromogenic reaction is quick and obvious in phenomenon, and the quick detection method is suitable for on-site quick detection.

Description

technical field [0001] The invention relates to the field of analytical chemistry detection, in particular to a rapid detection method for hydrocortisone. Background technique [0002] In recent years, people have paid more and more attention to health and drug safety. Because most of health care products and Chinese patent medicines are derived from natural substances, they have mild curative effects and high safety. They are favored by patients at home and abroad in the treatment of chronic diseases such as asthma. Favored, but it has the disadvantage of slow onset or inconspicuous effect. In order to make huge profits, some lawbreakers take advantage of people's eagerness to see results, and without any pharmacological and toxicological research, illegally add chemical drugs with fast onset and definite curative effects to them. Chemical drugs with antitussive effect are common now. There are theophylline, dexamethasone and so on. The chemical composition of health ...

Claims

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Application Information

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IPC IPC(8): G01N21/78
CPCG01N21/78
Inventor 李冰高辉
Owner SHANDONG INST FOR FOOD & DRUG CONTROL
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