Determination Of Sex-enhancing Drugs Illegally Added in Health Care Products By TLC-NIＲS Combined Technology Ⅱ

2. 4. 2 Model establishment

The study used the OPUS software that comes with the NIＲ spectrometer to preprocess the spectrum of each reference substance. Since the chemical component spectral information is affected by external noise, baseline drift, light scattering, background signal, temperature and humidity, the study used multiplication signal correction (MSC), vector normalization (VN), minimum maximum normalization (MMN), constant offset elimination (COE), first derivative (FD), second derivative (SD) and smoothing points (SP, smoothing points 5, 7, 9, 13, 17, 21, 25) filtering combination method to process the useless information in the spectrum and improve the accuracy of model discrimination, with the number of misjudgments of calibration set samples as the indicator (see Table 2).

 

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Based on the original spectrum preprocessing, the cursor is used to interactively select the spectral range with large differences; the standard algorithm-Euclidean distance (standard, STD) and factorization method-factor number (factorization, FC) calculation and analysis methods are used; the threshold (0.25) and confidence level are set

Fig. 6 TLC-NIＲS quantitative model of chemical drugs in health products

 

Table 5 TLC-NIＲS quantitative model of chemical drugs in health products

 

Environmental Factor	Predicted Ingredient	Predicted Range (µg µL⁻¹)	R²	RMSE (%)	RMSEP (%)
Western Viagra	Sildenafil	5.25 - 262.5	0.984	0.085	0.081
Eastern Viagra	Norc Sildenafil	5.15 - 257.5	0.982	0.078	0.075

 

 

2.5.5 Model validation and application

The above model was used to test 10 batches of sexual health samples and 10 batches of homemade sildenafil samples. The TLC-NIRS model prediction results were consistent with the HPLC content determination results. The R2 between the predicted values ​​and the measured values ​​of sildenafil and sildenafil were 0.982 and 0.996, respectively (see Figure 6); the average relative deviation of the predicted values ​​of 9 batches of sexual health samples was calculated to be 1.86%, and the average relative deviation of the predicted values ​​of 10 batches of homemade sildenafil samples was 1.96%, indicating that the model prediction results are accurate and reliable (see Table 6).

 

Table 6 TLC-NIＲS predicted values of 10 sex-enhancing products

 

Sample	Actual Value (mg/time)	Predicted Value (mg/time)	Absolute Deviation	Relative Deviation (%)	Mean Relative Deviation (%)
Gold flower extract	50.78	52.36	1.58	3.11	1.86
Insect repellent	50.36	52.48	2.12	4.21
German chamomile	77.20	78.58	1.38	1.79
Early morning dew	16.56	16.58	0.02	0.12
Wormwood	61.66	63.78	2.12	3.44
A. niger	45.20	45.98	0.78	1.73
Gold thread	Not detected	48.56	-	-

 

 

3 Conclusions

This study created the TLC-NIRS coupling technology for the first time because TLC is a classic traditional identification analysis method with the advantages of simple operation and wide popularity [12]. TLC has a large free space for sample processing. Different extraction solvents can be selected for the possible addition of prohibited chemical drugs, which can effectively avoid the influence of different manufacturers' products on NIRS due to different excipients; TLC has many optional materials, such as silica gel, alumina, polyamide, etc., and the developing agent can choose different polar reagents to be suitable for the separation and analysis of different types of chemical components. At the same time, different development systems can be used for bidirectional development, which has a good separation effect [12, 13], which can greatly improve the accuracy of NIRS collection of chemical drug information. NIRS is a rapid analysis instrument developed in recent years, with the characteristics of simple operation, fast analysis speed, and no chemical pollution [14]. This paper combines the advantages of each to create the TLC-NIRS coupling technology for the first time, and conducts a systematic methodological investigation of this method. A rapid qualitative and quantitative analysis model for the addition of banned chemical drugs sildenafil and nardenafil to health products was established.

The model was verified and evaluated using validation set samples. The qualitative model can better judge whether the above banned chemical drugs are added to health products, with a judgment accuracy of 100%; the quantitative model can accurately predict the content of added sildenafil and nardenafil, with a wide content prediction range of 5.25-262.5 and 5.15-257.5 μg/μL, respectively. The average relative deviations of the prediction results of 10 health products were 1.86% and 1.96%, respectively. The prediction results achieved good results and can meet the needs of actual rapid testing. In actual work, TLC-NIRS combined technology was used to crack down on multiple batches of sexual health products that added excessive doses of banned chemical drugs sildenafil.

This study selected nafil-like drugs as the research object because they are effective, cheap and easy to obtain in sexual health products, and are the first choice for illegal manufacturers to add them [3]. In addition, to achieve the expected effect, the effective dose of such sexual health drugs is 50-100 mg/time. Long-term overdose will cause serious liver and kidney damage and permanent loss of risk [18]. The use of TLC-NIRS model to predict whether nafil-like drugs are added to sexual health products has certain feasibility and research value.

This paper uses the existing analytical techniques and instruments on the current experimental platform for combined use, and has a good effect when applied to actual drug testing. The developed TLC-NIRS combined technology has a good application prospect in the face of problems such as uneven quality of health care product manufacturers, a wide variety of products, difficulty in unifying the source of excipients, and serious illegal additions.

The application theory and practical research of this combined technology provides a scientific basis for the development of TLC-NIRS combined instruments and equipment.

 

References

 

1 Conroy DM, Gan C, Errmann A, et al. Fortifying wellbeing: How Chinese consumers and doctors navigate the role of functional foods［J］． Appetite, 2021, 12: 105296．

2 Chen HZ, Gong JH. Innovating the concept of drug supervision and sampling inspection to crack down on illegal activities of illegally adding chemical substances in traditional Chinese medicine preparations［J］． Qilu Pharm Affairs, 2009, 28: 324-326. 3 Li K, Guo CC, Shi F, et al. Research progress in determination technologies for adulterated phosphodiesterase-5 (PDE5) inhibitors and their analogue in invigorant herbal medicines and dietary supplements［J］． Chin J Pharm Anal (Journal of Pharmaceutical Analysis), 2018, 38: 566-574.
4 Xu S, Jin PF, Xu QL, et al. Advances in the chemical substances illegally adulterated in traditional Chinese medicines and health foods［J］． Chin J New Drugs (Chinese New Drugs Journal), 2015, 24: 1843-1850．

5 Magdalene HY, Tang Sammy PL, Chen Sau W, et al. Case series on a diversity of illicit weight-reducing agents: from the well known to the unexpected［J］． British J Clin Pharm, 2011, 71: 250-253.

6 Kojima A, Sato Y, Chiba T, et al. Notable adverse events associated with concomitant use of health foods and drugs derived from the analysis of HFNet data on the safety and effectiveness of health foods［J］． J Food Hyg Soc Jpn, 2018, 59 (2): 80-88．