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Application of surface enhanced Raman spectroscopy to the determination of sibutramine in slimming tea

Launch:2023-10-10    

Research background

Sibutramine incident

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    In May 2020, the Public Security Bureau of Liaoyuan City, Jilin Province, found that sibutramine was contained in foods such as "slimming Monica" and "slimming S enzyme" being sold in a shopping mall in Liaoyuan City.

     The General Administration of Market Supervision reported that on May 16, 2020, the east police of Linyi River in Shandong Province destroyed a criminal chain for the production and sale of toxic and harmful weight loss products, involving more than 5 million yuan and confiscating 5 kilograms of sibutramine.

     In 2021, there was a heated discussion about the death of a 2-year-old child who accidentally ate a diet drug containing sibutramine.

What is sibutramine?

     Sibutramine is a mixed 5-HT and norepinephrine reuptake inhibitor, which was first used in the treatment of depression. Later, in clinical application, it was found that sibutramine has the effect of weight loss. Sibutramine can inhibit appetite by blocking the reuptake of norepinephrine and 5-HT, increase the glucose utilization and thermogenesis of adipose tissue, increase energy consumption and reduce body weight. Therefore, it was later used as a weight loss drug, and was approved to be listed in the United States in 1997 and in China in 2000.

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The harm of sibutramine

     However, with the in-depth study of sibutramine, it has been found that long-term use of weight-loss drugs or foods containing sibutramine can cause serious cardiovascular disease. Therefore, in 2010, the United States Food and Drug Administration recommended to stop the use of sibutramine, and sibutramine was subsequently withdrawn from international and domestic markets. On October 30, 2010, China officially suspended the production, sale and use of all preparations and APIs containing sibutramine, such as trimetidine and Nometine. However, due to the low price of sibutramine, and indeed has a certain effect of food inhibition and weight loss, it has been skillfully added by some unscrupulous businesses to make exorbitant profits in weight loss food.

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Sibutramine detection method

    At present, the determination methods of sibutramine in weight loss health products include spectrophotometry, high performance liquid chromatography, gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry and so on. However, most of the instruments used are expensive, the sample pretreatment time is long, and the comprehensive testing cost is high, so they are not suitable for rapid testing and mass sampling activities.

     In view of the shortcomings of current detection methods, such as sea photoelectricity combined with surface enhanced Raman technology, a Raman rapid detection kit for sibutramine in slimming tea was developed. This method has the advantages of simple operation, short detection time and low test cost. It can realize the detection of sibutramine in slimming tea in 20min to meet the rapid screening of sibutramine in slimming products.

Application case

Experimental object

Test substrate: a certain brand of slimming tea.

Test item: sibutramine.

Note: slimming tea samples have been tested by liquid chromatography-tandem mass spectrometry without sibutramine.

Instruments and consumables

Product

Model

Quantity

Box type Raman spectrometer

IRS1000

1

Pre-treatment one-piece box

RFSC-1000

1

Colorimetric dis

CVT-721

4

Sibutramine Raman rapid detection kit

/

1

Experimental scheme

     Before the beginning of this experiment, the slimming tea sample was detected by liquid phase-mass spectrometry to confirm that there was no sibutramine residue in the sample. The standard standard method is used to configure the samples to be tested in the following table, and the detailed experimental information is shown in the table below.

Experiment number

Experimental sample

Add drugs

Added concentration (mg/kg)

1

Slimming tea

--

--

2

Sibutramine

4
3

Sibutramine

6
4

Sibutramine

10

Testing method

     In this experiment, Oceanhood self-developed sibutramine Raman speed test kit combined with pre-processing machine was used for pre-treatment of slimming tea samples, box-type Raman spectrometer to collect spectral data, intelligence detection E + software for identification.

     Sample pretreatment process: weigh 1g of experimental sample, add extraction reagent, fully oscillate extraction. After extraction, it is purified by tea purification tube, and after purification, it is tested on the machine. For detailed testing process, please refer to the instructions of sibutramine Raman speed test kit.

Test result

     The test results of slimming tea samples with different concentrations of sibutramine are shown in the following figure. Compared with the blank tea samples without sibutramine, the Raman test spectra of tea samples with sibutramine have obvious Raman characteristic shift (1093cm-1). Comparing the test results of several tea samples with different concentrations of sibutramine, it was found that the corresponding Raman characteristic displacement intensity increased with the increase of sibutramine concentration. The intensity of the corresponding Raman characteristic peak at 1093cm-1 and the concentration of sibutramine were fitted, and there was a positive correlation and a good linear relationship between them, indicating that this method has a good testing effect on sibutramine in slimming tea.

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Conclusion

     The detection of sibutramine in slimming tea can be realized by such as Hesibutramine Raman rapid detection kit combined with pretreatment box and box type Raman spectrometer.