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Method for detecting dideacetylbisacoperidine and monodeacetylbisacoperidine

A technology for deacetylation and bisacodyl, which is applied in the detection of bisacodyl bisacodyl and monodeacetylbisacodyl, and in the field of chemical detection, and can solve problems such as lack of qualitative and quantitative detection methods.

Active Publication Date: 2020-05-29
苏州市药品检验检测研究中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to evade supervision, counterfeiters will mix these two compounds into weight loss products. A few days ago, it was found in the supervision and inspection of commercially available weight loss Chinese patent medicines and health food that these two ingredients were added, but there is no qualitative, Quantitative detection method

Method used

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  • Method for detecting dideacetylbisacoperidine and monodeacetylbisacoperidine
  • Method for detecting dideacetylbisacoperidine and monodeacetylbisacoperidine
  • Method for detecting dideacetylbisacoperidine and monodeacetylbisacoperidine

Examples

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Effect test

Embodiment 1

[0083] The detection method of bis-deacetylbisacodyl includes the following steps:

[0084] (1) Precisely weigh out 5 mg of the reference substance of di-deacetyl bisacodyl and mono-deacetyl bisacodyl, place them in a 50 mL volumetric flask, dissolve and dilute with methanol to the mark, as a stock solution; then pipette an appropriate amount , Dilute step by step with methanol to prepare a reference solution with a concentration of 2 ng / mL.

[0085] (2) Take 20 cellulose capsules (yellow capsules) of a certain batch number, pour the contents, mix evenly, weigh, weigh 1 powder of the contents, put it in a 50 mL volumetric flask, add methanol to 30 mL, vortex for 1 min, shake and extract for 30 min, stand still, add methanol to the mark, shake well, filter with 0.22 µm organic filter.

[0086] (3) Use ultra high performance liquid chromatography-linear ion trap mass spectrometry for qualitative screening: take blank solution, test solution and reference solution respectively, and inj...

Embodiment 2

[0105] The detection method of di-deacetyl bisacodyl and mono-deacetyl bisacodyl includes the following steps:

[0106] (1) Precisely weigh out 5 mg each of the di-deacetyl bisacodyl and mono-deacetyl bisacodyl reference substance, place them in a 50 mL volumetric flask, dissolve and dilute to the mark with methanol, as a stock solution; then pipette an appropriate amount, Dilute step by step with methanol to prepare a mixed reference solution with a concentration of 2 ng / mL.

[0107] (2) Take 20 slimming pink tablets of a certain batch, grind them to a particle size ≤180 μm, mix them evenly, weigh, weigh 1 piece of powder, place it in a 50 mL volumetric flask, add methanol to 30 mL, vortex Spin for 1 min, shake and extract for 30 min, stand still, add methanol to the mark, shake well, filter with 0.22 µm organic filter.

[0108] (3) Use ultra high performance liquid chromatography-linear ion trap mass spectrometry for qualitative screening. Take the blank solution, test solution an...

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Abstract

The invention provides a method for detecting dideacetylbisacodin and monodeacetylbisacodin. Qualitative screening, confirmation and content determination are carried out by adopting an ultra-high performance liquid chromatography-linear ion trap mass spectrometry method. Chromatographic conditions are as follows, a chromatographic column is a C18 chromatographic column, a detector is a linear iontrap, a mobile phase is A-0. 1% acetic acid solution and B-0. 1% acetic acid-methanol, the flow rate is 0.2 mL / min to 0.6 mL / min, the column temperature is 25-40 DEG C, the sample size is 0.1 to 5 [mu] L, an elution gradient program is carried out with 20%-90% of B for 0-5 min, 90% of B for 5-6min, 20% of B for 6.1-7min. The method can be used for exclusively, sensitively and quickly primarily screening and confirming the dideacetylbisacodin and the monodeacetylbisacodin which are added into the weight-reducing Chinese patent medicines and health-care foods, and is mainly suitable for analyzing Chinese patent medicines and the health-care foods in solid dosage forms.

Description

Technical field [0001] The invention belongs to the field of medical detection, and relates to a detection method of chemicals, in particular to a detection method of di-deacetyl bisacodyl and mono-deacetyl bisacodyl. Background technique [0002] Bisacodyl is a contact laxative that stimulates sensory nerve endings through direct contact with the intestinal mucosa, causing increased intestinal reflex peristalsis and leading to defecation. Because this medicine has a certain slimming effect, it is added to weight-loss Chinese patent medicines and health foods by illegal merchants, which is harmful to the health of consumers. At present, the national legal inspection standard (Determination of sibutramine and other compounds in food BJS 201701) has included the detection method of bisacodyl, which is a prohibited ingredient. [0003] Two analogues of bisacodyl: bis-deacetylbisacodyl (CAS number: 603-41-8, molecular formula: C 18 H 15 NO 2 , Molecular weight: 277.1) and monodeacetyl...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/72G01N30/86
CPCG01N30/02G01N30/06G01N30/34G01N30/72G01N30/8634
Inventor 贾昌平郑佳新郑梅陈丽波钱叶飞赵琪张珊珊张斌储蓉
Owner 苏州市药品检验检测研究中心
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