ILLICIT Drug Identification: HPLC Analysis Case Study

ILLICIT Drug Identification: HPLC Analysis

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Introduction: ILLICIT Drug Identification: HPLC Analysis

In this chapter, the lab report is based on the identification of illicit drugs that are used by males aged 18 and 22. To identify the powder the laboratory test is important. The objectives of the study are discussed here. The main objectives are-

• To identify the illicit drug, the lab technician will have to use “high-performance liquid chromatography” or HPLC. The identification of the drugs should primarily be based on “retention time,” which is calculated in the laboratory.
• To create a standard calibration set. This is important for the calculation of the amount of the drug. The drug will have to be used as a diluted sample. From the calculated and observed graph, the “peak areas” of the graphs will have to be observed, and based on these peak areas the quantification of the drug should have to do. The % purity of the samples will have to be calculated.
• To report the analytical data that is collected in the laboratory. The data have to be collected based on ATR-FTIR spectroscopy in the laboratory. The reflectance of the FTIR spectroscopy will have to be calculated.

Materials and methods

Materials or reagents that are used in this experiment

Reagents	Amount of reagents
Cocaine standard	1 mg/mL
Ketamine standard	1 mg/mL
Benzocaine standard	1 mg/mL
Unknown sample’s extract	1 mg/mL

In the above chart, the reagents that are used in the laboratory for this experiment are discussed. The above-mentioned reagents will have to be used in the mobile phase that is used in the HPLC experiment of chromatography.

Methods that are used in the experiment

• The syringe of injection in which the diluted sample will have to take for the experiment will have to be rinsed first, with the help of deionized water. After rinsing the sample will have to be injected into the instrument of HPLC.
• The above-mentioned step will have to carry forward for each of the three unknown samples. In this case, the three samples are cocaine, benzocaine, and ketamine. The lab technician will have to be identified the samples between these three samples. The instrument that is important for the experiment will have to be ready before the injection of the unknown samples.
• The chromatograms of the samples will have to be collected. After the collection process is done then the lab technician will have to make notes about the column type, HPLC manufacturer, the composition of the mobile phase, and the wavelength of the detector will also have to be calculated.
• After the above steps, the analysis of the chromatograms will have to be done. Then the components can be identified with the help of a chromatogram.
• Then the illicit drug will have to be identified.
• A standard calibration set will have to be produced.
• Then a calibration curve will have to be determined.

Concentration (microgram/mL)	The volume of stock of solution (mL)	The volume of deionized water (mL)	Final volume (mL)
0	0	1	1
25	0.25	0.75	1
50	0.50	0.50	1
75	0.75	0.25	1
100	1	0	1

Table 1: A standard calibration table

Result and discussion

Figure 1: HPLC chromatogram for an unknown sample

From the chromatogram it is observed that the retention time for the highest peak is 4.968 min. The area of the highest peak is 6240.44 mAU and the height of the highest peak is 469.13nm. The wavelength used in the chromatogram is 217 nm.

RT [min]	Area	Height	Area %
2.578	156.65	37.04	2.37
2.787	120.45	26.33	1.82
3.399	41.87	8.80	0.63
4.968	6240.44	469.13	94.31
5.771	19.78	2.39	0.30
9.436	37.94	3.45	0.57

Table 2: Report of the chromatogram

Figure 2: HPLC chromatogram for unknown sample

From the chromatogram it is observed that the retention time for the highest peak is 4.916 min. The area of the highest peak is 8232.53 mAU and the height of the highest peak is 557.55nm. The wavelength used in the chromatogram is 217 nm.

RT [min]	Area	Height	Area %
2.573	221.47	48.25	2.54
2.780	134.91	27.56	1.55
3.392	47.67	10.49	0.55
4.916	8232.53	557.55	94.43
5.760	28.46	3.22	0.33
9.433	53.08	4.21	0.61

Table 3: Report of the chromatogram

Figure 3: HPLC chromatogram for unknown sample

From the chromatogram it is observed that the retention time for the highest peak is 5.013 min. The area of the highest peak is 4315.04 mAU and the height of the highest peak is 375.20nm. The wavelength used in the chromatogram is 217 nm.

RT [min]	Area	Height	Area %
2.216	24.54	2.63	0.53
2.585	135.50	32.49	2.94
2.792	81.26	17.81	1.76
3.406	36.36	7.41	0.79
5.013	4315.04	375.20	93.51
5.780	22.05	2.52	0.48

Table 4: Report of the chromatogram

Figure 4: HPLC chromatogram for an unknown sample

From the chromatogram it is observed that the retention time for the highest peak is 4.953 min. The area of the highest peak is 6297.40 mAU and the height of the highest peak is 474.92nm. The wavelength used in the chromatogram is 217 nm.

RT [min]	Area	Height	Area %
2.580	210.05	46.85	3.13
2.786	116.24	25.83	1.73
3.398	57.31	11.38	0.85
4.953	6297.40	474.92	93.81
9.412	32.15	2.85	0.48

Table 5: Report of the chromatogram

Figure 5: HPLC chromatogram for unknown sample

From the chromatogram it is observed that the retention time for the highest peak is 3.714 min. The area of the highest peak is 24.76 mAU and the height of the highest peak is 1.48nm. The wavelength used in the chromatogram is 217 nm.

RT [min]	Area	Height	Area %
3.714	24.76	1.48	100.00

Table 6: Report of the chromatogram

Figure 6: HPLC chromatogram for unknown sample

From the chromatogram it is observed that the retention time for the highest peak is 5.011 min. The area of the highest peak is 4448.70 mAU and the height of the highest peak is 381.15 nm. The wavelength used in the chromatogram is 217 nm.

RT [min]	Area	Height	Area %
2.211	30.81	3.96	0.65
2.585	137.28	33.04	2.88
2.793	83.72	17.61	1.76
3.407	40.64	7.63	0.85
5.011	4448.70	381.15	93.29
9.420	27.29	2.46	0.57

Table 7: Report of the chromatogram

Figure 7: HPLC chromatogram for unknown sample

From the chromatogram it is observed that the retention time for the highest peak is 2.133 min. The area of the highest peak is 14858.35 mAU and the height of the highest peak is 2870.16 nm. The wavelength used in the chromatogram is 217 nm.

RT [min]	Area	Height	Area%
2.133	14858.35	2870.16	99.24
5.235	49.23	4.81	0.33
6.832	22.18	1.34	0.15
7.971	19.23	1.32	0.13
9.550	23.51	1.47	0.16

Table 8: Report of the chromatogram

Figure 8: HPLC chromatogram for unknown sample

From the chromatogram it is observed that the retention time for the highest peak is 2.211 min. The area of the highest peak is 21917.63 mAU and the height of the highest peak is 3737.87 nm. The wavelength used in the chromatogram is 217 nm.

RT [min]	Area	Height	Area %
2.211	21917.63	3737.87	100.00

Table 9: Report of the chromatogram

Conclusion

After the analysis of the above data it is clear that the time of retention for cocaine peaks at 4.916 min. The retention time for ketamine is 2.133, and for benzocaine is 2.211 min. The time of retention for the unknown sample is 4.968 min. The wavelength used in the chromatogram is 217 nm. The reflectance of the FTIR spectroscopy will have to be calculated.

References

Book

DG Watson, 2020 Pharmeceutical Analysis Available at http://repository.UKbooks.id/id/eprint/275/1/MCU_2017_Pharmaceutical_Analysis_A_Textbook_for_Pharmacy_Students.pdf [Accessed on 12.04.2023]

Journal

D'Odorico, P., Schönbeck, L., Vitali, V., Meusburger, K., Schaub, M., Ginzler, C., Zweifel, R., Velasco, V.M.E., Gisler, J., Gessler, A. and Ensminger, I., 2021. Drone?based physiological index reveals long?term acclimation and drought stress responses in trees.Plant, Cell & Environment,44(11), pp.3552-3570.

Farrar, M.B., Wallace, H.M., Brooks, P., Yule, C.M., Tahmasbian, I., Dunn, P.K. and Hosseini Bai, S., 2021. A performance evaluation of vis/nir hyperspectral imaging to predict curcumin concentration in fresh turmeric rhizomes.Remote Sensing,13(9), p.1807.

Frioni, T., Squeri, C., Del Zozzo, F., Guadagna, P., Gatti, M., Vercesi, A. and Poni, S., 2021. Investigating evolution and balance of grape sugars and organic acids in some new pathogen-resistant white grapevine varieties.Horticulturae,7(8), p.229.

Liu, K., Huang, S., Jin, Y., Ma, L., Wang, W.X. and Lam, J.C.H., 2022. A green slurry electrolysis to recover valuable metals from waste printed circuit board (WPCB) in recyclable pH-neutral ethylene glycol.Journal of Hazardous Materials,433, p.128702.

Luo, J., Li, M., Wu, H., Liu, Z., Barrow, C., Dunshea, F. and Suleria, H.A., 2022. Bioaccessibility of phenolic compounds from sesame seeds (Sesamum indicum L.) during in vitro gastrointestinal digestion and colonic fermentation.Journal of Food Processing and Preservation,46(7), p.e16669.

Zhu, L., Zhao, Y., Liu, T., Chen, M., Qian, W.P., Jiang, B., Barwick, B.G., Zhang, L., Styblo, T.M., Li, X. and Yang, L., 2022. Inhibition of NADPH oxidase-ros signal using hyaluronic acid nanoparticles for overcoming radioresistance in cancer therapy.ACS nano,16(11), pp.18708-18728.

Article

Orsolini, L., Corkery, J.M., Chiappini, S., Guirguis, A., Vento, A., De Berardis, D., Papanti, D. and Schifano, F., 2020. ‘New/designer benzodiazepines’: an analysis of the literature and psychonauts’ trip reports.Current neuropharmacology,18(9), pp.809-837. Accessed from https://www.unodc.org/documents/scientific/STNAR47_Piperazines_Ebook.pdf [Accessed on 12.04.2023]