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Method for detecting ephedrine additives doped in weight-losing traditional Chinese medicines

A technology of ephedrines and additives, which is applied in the field of medical analysis, can solve the problems of poor accuracy, inability to develop color, and large volume, and achieve the effects of avoiding false positive or false negative results, simple and fast detection process, and simple experimental operation

Active Publication Date: 2015-09-30
SECOND MILITARY MEDICAL UNIV OF THE PEOPLES LIBERATION ARMY
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  • Abstract
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AI Technical Summary

Problems solved by technology

By TLC method, the standard substance of the Chinese medicine to be tested and four kinds of ephedrine additives is subjected to thin-layer chromatography through an appropriate developer, and the ratio shift value (Rf value) is compared to determine that the weight loss Chinese medicine is mixed with ephedrine additives , although this method is simple and quick, but the accuracy is poor, and the test results are easily affected by other ingredients in the weight-loss traditional Chinese medicine, and the ultraviolet absorption of the ephedrine additives is poor, and when the content is small, the color cannot be developed on the TLC plate. It is easy to cause misjudgment, false positive or false negative results
Although the detection results of HPLC method and HPLC-MS method are accurate and reliable, they need to be completed after tedious pretreatment of the sample, so it takes a lot of time, and the instrument is expensive and bulky. When testing traditional Chinese medicine, the HPLC method and HPLC-MS method not only need to prepare relevant mobile phases and gas pipelines, but also have very strict requirements on the experimental conditions and venues. Therefore, it is difficult to use them in on-site quick testing

Method used

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  • Method for detecting ephedrine additives doped in weight-losing traditional Chinese medicines
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  • Method for detecting ephedrine additives doped in weight-losing traditional Chinese medicines

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Embodiment 1

[0035] In this embodiment, the equipment used includes: a portable Raman spectrometer (BWS415, B&W Tek Inc., the United States), with an excitation wavelength of 785nm and a resolution of 5cm -1 , spectral coverage 175-3200cm -1 ; WFH-203B three-purpose ultraviolet analyzer (Shanghai Jingke Industrial Co., Ltd.); ultrasonic instrument (KUDOS-SK5200HP, China); centrifuge (HERAEUS, FRESCO17Centrifuge; Thermo Scientific, USA); analytical balance (METTLER AE240, China).

[0036]In this embodiment, the materials used include: thin-layer board GF254 (coating thickness: 0.2mm±0.03mm, silica gel powder particle size: (8±2)m≧80%), Yantai Jiangyou Silica Gel Development Co., Ltd.); Silver nitrate and trisodium citrate (AR, Sinopharm Chemical Reagent Co., Ltd.); other reagents used were of analytical grade, purchased from Sinopharm Chemical Reagent Co., Ltd.; chromatographically pure formic acid was purchased from Tedia (USA); mass spectrometrically pure methanol was purchased from Fish...

Embodiment 2

[0056] Adopt the equipment and the material that embodiment one provides, the surface enhancer that adopts is silver sol, the method that provides detects the method for doping ephedrine additives in weight-reducing traditional Chinese medicine is carried out in portable Raman spectrometer, and the Raman spectrum that obtains The figure uses standard spectrum processing software to process the non-blank spectrum, including selecting 300cm -1 ~1700cm -1 The spectral segment was smoothed by the Sgolay method and baseline corrected by the airPLS method to obtain a preprocessed surface-enhanced Raman spectrum. A weight-loss traditional Chinese medicine to be checked is as follows: take an appropriate amount of the weight-loss Chinese medicine to be checked in Example 1, grind it finely, divide it into four parts, and use it as a negative sample; accurately weigh ephedrine, pseudoephedrine, methylephedrine and demethylephedrine Alkaline reference substances were added to each nega...

Embodiment 3

[0083] When it is determined that the weight-loss traditional Chinese medicine is doped with ephedrine additives, the pretreatment surface-enhanced Raman spectrum should continue to be judged as follows:

[0084] When the surface-enhanced Raman spectrum of pretreatment is at 753±10cm -1 If there is an absorption peak at the place, it is determined that there is ephedrine doped in the weight loss Chinese medicine to be tested;

[0085] When the surface-enhanced Raman spectrum of pretreatment is at 713±10cm -1 , 738±10cm -1 and 768±10cm -1 If there are absorption peaks in at least two of the three peak positions, it is determined that pseudoephedrine is doped in the weight loss Chinese medicine to be tested;

[0086] When the surface-enhanced Raman spectrum of pretreatment is at 469±10cm -1 , 724±10cm -1 , 829±10cm -1 , 892±10cm -1 , 1133±10cm -1 and 1236±10cm -1 If there are absorption peaks at least five of the six peak positions, it is determined that methylephedrine...

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Abstract

The invention discloses a method for detecting ephedrine additives doped in weight-losing traditional Chinese medicines. The method comprises the following steps: carrying out thin layer chromatography on weight-losing traditional Chinese medicines to be detected; dropwise adding a surface reinforcing agent at the four positions with Rf values being 0.30-0.33, 0.34-0.36, 0.37-0.39 and 0.50-0.53, and scanning the four positions by adopting a portable raman spectrometer to obtain four original surface enhanced raman spectrograms, when the four original surface enhanced raman spectrograms are blank spectrograms, determining that the weight-losing traditional Chinese medicines to be detected do not contain ephedrine additives, and when the four original surface enhanced raman spectrograms contain non-blank spectrograms, processing the non-blank spectrograms to obtain preprocessed surface enhanced raman spectrograms; and when the preprocessed surface enhanced raman spectrograms contain at least five absorption peaks of ephedrine additives, determining that the weight-losing traditional Chinese medicines are doped with ephedrine additives, otherwise, determining that the weight-losing traditional Chinese medicines do not contain the ephedrine additives. According to the method, the technical solution has high accuracy, field detection can be implemented, a reference substance is not needed, the application range is wide, the operation is simple, and the cost is relatively low.

Description

technical field [0001] The invention relates to a method for detecting ephedrine additives doped in traditional Chinese medicine for weight loss, and belongs to the technical field of medical analysis. Background technique [0002] Because weight-loss traditional Chinese medicine has mild effect and little side effect compared with weight-loss western medicine, it is therefore more and more favored by beauty lovers. However, traditional Chinese medicine usually takes a slow effect. In order to make their products have significant curative effect and rapid onset, some unscrupulous manufacturers mix ephedrine additives with weight loss effect into weight loss traditional Chinese medicine, such as ephedrine. In order to avoid being detected, there are even more What's more, its analogues such as pseudoephedrine, methylephedrine, and demethylephedrine are added to seek illegal gains. [0003] These ephedrine analogues can cause rapid heartbeat and vasoconstriction in users. The...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/65
Inventor 陆峰吕狄亚娄子洋柴逸峰曹岩李皓朱青霞李丹
Owner SECOND MILITARY MEDICAL UNIV OF THE PEOPLES LIBERATION ARMY
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