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Detecting method and kit of sibutramine hydrochloride

A technology of sibutramine hydrochloride and a 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. Long processing time, high analysis cost, high detection specificity, simple and fast operation, and obvious color changes.

Inactive Publication Date: 2013-09-04
WUXI ZODOLABS BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages are: (1) The chromatographic resolution is low, the ingredients of traditional Chinese medicine preparations are complex, and there are many interference factors. It is easy to misjudge some coexisting ingredients as sibutramine hydrochloride. The proximity of sibutramine will interfere with the detection of target components
(2) The time for chromatographic development and drying is long, which cannot meet the requirements of rapid determination
(3) Thin-layer chromatography plates need to be paved, dried and stored dry (prefabricated thin-layer chromatography plates need to be stored dry), and the ambient temperature and humidity have a great influence on the separation effect
(5) A fixed experimental site is required, and it is not suitable for on-site testing with high mobility
Its disadvantages are: (1) The instrument is expensive, and the sample pretreatment time is long. Most of them are for a single product, and the mobile phase used is mostly a certain proportion of methanol and salt solution. Contaminated, high analysis cost; (2) When the chromatographic retention time of the coexisting components is close to that of sibutramine hydrochloride, it is easy to make a wrong judgment; (3) The instrument has high requirements for the use environment and needs to be fixed. Not suitable for on-site testing with high mobility
These tests can only be carried out in a small number of laboratories and are not easy to promote and use

Method used

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  • Detecting method and kit of sibutramine hydrochloride
  • Detecting method and kit of sibutramine hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] The detection of embodiment 1 capsule

[0041] Sample: Qumei Qingmeishuang Slimming Capsules (capsules, the labeled dosage is 2 capsules each time, as determined by high performance liquid chromatography, each capsule of this product contains 5.90 mg of sibutramine hydrochloride).

[0042] Detection steps:

[0043]Take 1 sample, put its contents (about 0.4g) into a 10mL sample bottle, add 5mL of acetonitrile solvent, shake and mix well, let stand for two minutes, filter, and collect the filtrate. Add 3mL of 0.1mmol / L hydrochloric acid solution to the filtrate, mix well, place to separate layers, take about 2mL of the extract from the lower layer into a 10mL colorimetric tube, add 0.1mL of B-R buffer solution with pH 3.70, and 1.5mL of bromophenol blue color developer , the color immediately turns blue, which means that Qumeiqingmeishuang Slimming Capsules contain sibutramine hydrochloride.

Embodiment 2

[0044] The detection of embodiment 2 tablet

[0045] Sample: Natural Meilai Apple Cider Vinegar Slimming Tablets (tablets, the labeled dosage is 2 tablets each time, and the results of high performance liquid chromatography determine that each tablet of this product contains 14.79mg of sibutramine hydrochloride).

[0046] Take 1 piece of sample (about 0.4g), grind it evenly, put it in a 10mL sample bottle, add 5mL of methanol solvent, shake and mix evenly, let stand for two minutes, filter, and collect the filtrate. Add 3mL of 0.05mmol / L sulfuric acid solution to the filtrate, mix well, place to separate layers, take about 2mL of the extract from the lower layer and put it in a 10mL colorimetric tube, add 0.1mL of B-R buffer solution with pH 3.00, and 1.5mL of bromophenol blue color developer , the color immediately turned blue, and the absorbance was detected at 436nm. According to the standard curve, the accurate content was measured to be 14.90 mg, which means that Sibutram...

Embodiment 3

[0048] Example 3 Detection of tea preparation

[0049] Sample: Miele brand slimming portable tea (tea preparation, the labeled dosage is 1 pack each time, and the product does not contain sibutramine hydrochloride as determined by high performance liquid chromatography).

[0050] Detection steps:

[0051] Take about 0.5g of the sample, put it in a 10mL sample bottle, add 5mL of ethanol solvent, shake and mix well, let stand for two minutes, filter, and collect the filtrate. Add 3mL of 0.2mmol / L phosphoric acid solution to the filtrate, mix well, place to separate layers, take about 2mL of the extract from the lower layer into a 10mL colorimetric tube, add 0.1mL of B-R buffer solution with pH 4.00, and 1.5mL of bromophenol blue color reagent , the solution is still yellow, that is to say, Miele brand slimming portable tea does not contain sibutramine hydrochloride.

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Abstract

The invention discloses a quick detecting method of sibutramine hydrochloride. The method sequentially comprises the following steps of: (1) extracting sibutramine hydrochloride from a sample through an organic solvent; (2) extracting and purifying the sibutramine hydrochloride through an inorganic acid solution; and (3) adding bromophenol blue as an indicator, and judging the result through chromogenic reaction. The invention further provides a special detecting kit of the method. The kit comprises one or a mixed solution of methanol, ethanol, n-butyl alcohol, dichloromethane and acetonitrile, the inorganic acid solution, and the bromophenol blue solution. Compared with the prior art, the method disclosed by the invention is low in analysis cost, free of special equipment, strong in specificity, high in sensitivity, and simple, convenient and quick to operate, thereby being suitable for onsite inspection. The quick detecting kit of sibutramine hydrochloride prepared by the method can meet the demands of related food supervision and inspection in extensive rural areas.

Description

technical field [0001] The invention relates to a detection method and a detection kit of sibutramine hydrochloride. Background technique [0002] Sibutramine Hydrochloride (English name is Sibutramine Hydrochloride), its chemical formula is: (±)1-(4-chlorophenyl)-N,N-dimethyl-2-(2-methylpropyl)-cyclo Butylmethylamine hydrochloride monohydrate is a tertiary amine compound. Molecular formula: C17H26ClN HCl H2O, structural formula: [0003] . [0004] In recent years, due to the improvement of human material life and the unreasonable diet structure, the number of people with obesity is on the rise year by year. Obesity can induce or aggravate diabetes, fatty liver, cardiovascular and cerebrovascular diseases, sleep apnea syndrome, etc. It has become a major enemy affecting human health and longevity, and has attracted more and more attention. Therefore, weight loss medicine has come into people's life. Weight loss drugs are mostly appetite suppressants that act on the c...

Claims

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Application Information

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IPC IPC(8): G01N21/78G01N1/28
Inventor 卞禹卜陶艳伟卫喜燕杨晓慧李林
Owner WUXI ZODOLABS BIOTECH
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