Drug Samples Research Articles

Development and characterization of a copolymeric micelle containing soluble and insoluble model drugs.

Micelles are nano-sized particles with a core-shell structure that are made by natural or synthetic polymers or copolymers. The aim of this study was to develop and characterize a copolymeric micelle using two polymers loaded with hydrophilic and lipophilic drugs. Poly(ethylene glycol) and poly(ε-caprolactone) (PEG-PCL) were used to form a copolymeric micelle which was further loaded with either moxifloxacin or clarithromycin as hydrophilic and lipophilic drug samples, respectively. Characterization tests were done including fourier transform-infrared (FT-IR) spectroscopy, proton nuclear magnetic resonance (1H NMR) spectroscopy, encapsulation efficiency, particle size, zeta potential, polydispersity index, transmission electron microscopy, and in-vitro release test. The construction of the copolymer was confirmed by the results of FT-IR and 1H NMR spectroscopy tests. The encapsulation efficiency test exhibited that loading was about 50% for twelve formulations. Particle size, zeta potential, polydispersity index, and transmission electron microscopy confirmed the formation of monodispersed, uniform, and nano-sized micelles with a few negative charges. The kinetic model of release was fitted to the Higuchi model. Polymeric micelles consisting of PEG-PCL copolymer were loaded with adequate concentrations of hydrophilic (moxifloxacin) and lipophilic (clarithromycin) model drugs, with a mean particle size under 300 nm. Therefore, copolymeric micelles can be used as a suitable drug delivery system for mucous membranes and skin.

Necrotic Upper-Extremity Infections in People Who Inject Drugs: A Case Series

Our institution has noted an increase in severe upper-extremity infections within the last 2 years. These patients have required transhumeral amputation. This case series demonstrates some of the catastrophic outcomes of these infections in people who inject drugs, which has been postulated to be related to the addition of xylazine to injectable drugs in our community. The study included patients presenting with severe upper-extremity infections resulting from intravenous drug use and requiring upper-extremity amputation between January 1, 2020 and September 30, 2022 at a single, urban, level 1 trauma center. Patient information and clinical images were collected through retrospective chart review. Eight patients were identified at our institution with extensive necrosis of the skin and soft tissues in the forearm and hand, resulting in exposure of the radius and ulna. None of these patients had viable motor function in the hand and presented with a lack of sensation. All underwent transhumeral amputations, including bilaterally in one case. The patients in this case series self-reported injection of tranquilizer-containing drugs, and xylazine has been reported to be present in 91% of heroin and fentanyl samples in our community. Although more studies are needed to confirm that xylazine is the definitive cause of the extensive tissue necrosis seen in these patients, we have found the severity of these infections to be noteworthy, given the likely expansion of xylazine to drug samples beyond our region. Therapeutic V.

Validated method for the analysis of 22 illicit drugs and their metabolites via liquid chromatography tandem mass spectrometry (LC-MS/MS) in illicit drug samples collected in Chicago, IL.

Drug checking services are being utilized worldwide to provide people who use drugs information on the composition and contents of their drugs as a tool for harm reduction and accidental overdose prevention. Existing drug checking services use a variety of techniques including immunoassay strips and spectroscopic techniques like FTIR and Raman. Few services utilize LC-MS based methods for primary or secondary analysis and few methods exist for direct analysis of illicit drugs. To address this, an LC-MS/MS method was developed for 22 illicit drugs and cutting agents using LC-MS/MS with application to 124 illicit drug samples that were collected from Chicago, IL. Samples were also analyzed using fentanyl and benzodiazepine immunoassay test strips. Fentanyl test strips gave a positive result for 86% of samples with only one sample showing a positive result on a benzodiazepine test strip. LC-MS/MS analysis of samples show that opioids were the most commonly quantified in 96% of samples, followed by stimulants at 12% and benzodiazepines at 1%. Fentanyl was measured in 91% of samples, co-occurring with heroin in 58% of opioid-containing samples. A comparison of the gold-standard LC-MS/MS results to fentanyl test strips shows a high level of accuracy for the fentanyl test strips, with just 5% of samples being classified as false negatives and no false positives. These results demonstrate the strengths and benefits of LC-MS/MS when incorporated as a secondary analysis tool for drug checking.

Development and validation of a rapid GC–MS method for seized drug screening

Controlled substances are one of the most commonly analyzed types of evidence in forensic laboratories. Persistent, high levels of case submissions in recent years have created a need for rapid screening techniques to decrease case backlogs and expedite confirmatory analyses. The most utilized technique for the analysis of seized drugs is gas chromatography mass spectrometry (GC-MS). While this approach typically takes tens of minutes, advances in the technique have enabled approximately 1 min run times with a short column and a rapid (10’s °C/s) temperature program. These advances were used in this work to develop and validate a rapid GC-MS method for screening seized drug samples. Method validation was completed to determine retention time repeatability and reproducibility, limits of detection, identification accuracy, selectivity, and carryover. Validation results showed the utility of this method for accurate and precise qualitative analyses for the screening of seized drugs across seven different drug classes. The optimized method was then applied to 15 real and mock case samples from the Maryland State Police Forensic Sciences Division. Controlled substances, cutting agents, and other diluents were identified from these samples using acceptance criteria of retention time and mass spectral comparisons currently used in casework. Using rapid GC-MS methods in casework could enable faster and more reliable presumptive testing results for the analysis of seized drug exhibits.

Study of the influence of ingredients on biopharmaceutical factors and pharmacological activity of a medicinal product with carrot extract and rutin

Aim. The work aimed to study the influence of the components of a soft rectal medicine with carrot root extract and rutin on biopharmaceutical parameters and its pharmacological activity.
 Materials and methods. The objects of the study were samples of soft pharmaceutical forms made on different bases. Pharmacological, biopharmaceutical, physicochemical and pharmacotechnological research methods were used in the study.
 The results. According to the data of organoleptic studies, determination of colloidal stability, and determination of pH, it was established that the studied samples were stable during the entire observation period. According to the data of rheological studies, it was established that all systems are thixotropic. However, the recovery time of the system is different, which is related to the physicochemical properties of auxiliary substances included in the samples. The performed spectral analysis of dialysate solutions of experimental samples of soft medicine indicates the possibility of quantitative determination of the number of flavonoids in dialysates in terms of rutin. The components of the base of the samples and the thick extract of carrot roots do not interfere with the determination of rutin in dialysates with pH 6.8 by the absorption spectrophotometry method at a wavelength of 352 nm. The analysis of the obtained results of the study of the release of rutin from samples into a phosphate buffer solution by dialysis through a semipermeable membrane shows that the complete release is provided by auxiliary substances used in the preparation of sample No. 4, which is an emulsion of the first kind. The obtained data from pharmacological studies on the dynamics of planimetric indicators on the model of stencil wounds in rats demonstrated a wound-healing effect in all the studied samples and the reference agent - Hemorol suppositories. However, using sample No. 4 in the treatment of a stencil wound promotes faster healing, which in clinical use can contribute to reducing the risk of infection, the spread of infection, and reducing the area of ​​the wound defect.
 Conclusions. According to the results of the complex studies, moderate advantages of sample No. 4 over the comparison drug and other samples have been established, determining the perspective of further research

A UV Spectrophotometric Assay of Extended-Release Brands of Etodolac

A simple, novel, economical and less time taking UV Spectrophotometric analysis was developed for Etodolac. The assay is relied on measuring optical density at lambda maximum 224.80nm wavelength using methanol as solvent. Four different brands of etodolac i.e. Etofree-ER (A), Toldin-ER (B), Etova-ER (C) and) Musran- ER (D) were procured from local market for analysis. The Drug sample was dissolved in methanol to get a concentration of 5μg/ml and its absorbance was measured. Similarly the samples of different brands were prepared in methanol with concentration range of 1-5μg/ml and their absorbance was recorded at 224.80nm following blank. The Assay percentage is being calculated and regression analysis is performed. The brand Etofree-ER (A) and Musran- ER (D) showed nearly same % Assay values i.e. 108.01% and 108.13% respectively. The brands Toldin-ER (B) and Etova-ER showed 105.42% and 106.84% Assay values. All the brands % Assay values were found to be with in limit as per Indian Pharmacopeia and their squared correlation co-efficient was also found to be 0.999 well within the limit.

Stability for 6 months and accuracy of a specific enteral caffeine base preparation for a multisite clinical trial.

The 'Intermittent Hypoxia and Caffeine in Infants Born Preterm (ICAF)' study (NCT03321734) uses an extemporaneously compounded enteral caffeine base solution for its study drug. The primary aim of this report is to determine the stability of this specific enteral caffeine base preparation stored for up to 6 months and assess optimal storage temperature. To analyse stability, caffeine solutions were prepared and stored at 4°C and 25°C (room temperature). The caffeine concentrations were analysed over time using high-performance liquid chromatography (HPLC). To confirm the accuracy of compounded caffeine concentrations, study drug samples from three research pharmacies were analysed. Stability results showed that caffeine concentrations are within 5% of the expected concentration when stored for up to 6months at room temperature. Our results also show that accurate caffeine concentrations were achieved by multiple research pharmacies.

The Canadian Psychedelic Survey: Characteristics, Patterns of Use, and Access in a Large Sample of People Who Use Psychedelic Drugs

The Canadian Psychedelic Survey: Characteristics, Patterns of Use, and Access in a Large Sample of People Who Use Psychedelic Drugs

RP-HPLC Method Development and Validation for Simultaneous Estimation of Escitalopram Oxalate and Atazanavir Sulphate in Bulk and Dosage Form

Background: This study was designed for the estimation of escitalopram oxalte and atazanavir sulphate in the experimental tablet formulation. The separation was performed at 210 nm by using Inertsil ODS 3V (250 * 4.6 mm, 5.0 m) column and acetonitrile/phosphate buffer (pH =3.55) as the eluent under isocratic elution conditions at a flow rate of 1.0 mL/min. Results: Escitalopram oxalate and atazanavir sulphate peaks were eluted at 2.636 and 3.319 minutes and no interference was observed in the diluent blank at the respective retention times, indicating that the developed method was specific and selective. A linear relationship was found for escitalopram oxalte (2.5 - 15 µg mL-1) and atazanavir sulphate (30 - 150.0 µg mL-1), with coefficient of regression greater than 0.999. Based on the RSD values (< 2.0%) and recovery results (> 98%), the developed method is accurate. At room temperature and in the refrigerated conditions, standard and sample solutions of escitalopram oxalate and atazanavir sulphate have been found to be stable for 48 hours. Conclusion: The established method is linear, precise, accurate, specific, and robust in the studied concentration range. Accordingly, the proposed method can be applied to the analysis of experimental tablet formulations as well as bulk drug samples.

Abstract LB162: A multiplex organoid avatar drug testing platform for precision medicine

Abstract The promise of precision medicine is to improve patient outcomes by making better therapeutic choices based on cancer causing somatic mutations. This strategy has shown limited success in colorectal cancer, in part because the genetic rules governing resistance and sensitivity are not fully elucidated. Direct drug sensitivity testing of individual patient-derived organoids is an attractive addition to this decision process because it does not require understanding of all drug-somatic mutation interactions. Individual patients avatars can be challenged with a variety of drugs and response used to inform patient care. We have developed a panel of colon cancer organoid avatars and uniquely tagged each one with a lentiviral vector possessing identifying DNA sequence bar codes flanked by common PCR primers. Each bar-code is uniquely identifiable and quantifiable from a mixture of organoids by nanopore sequencing of a common PCR product. Treatment of the mixture of organoid avatars over time under multiple drug conditions and sampling at different time points allowed the real-time monitoring of relative Darwinian fitness of each organoid in the mixture. We demonstrated the utility of this approach at identifying both expected and novel drug responses for individual organoids. Resistance to both nutlin and irinotecan were correctly predicted by TP53 somatic mutations while sensitivity to both lapatinib and ibrutinib were best predicted by mutations in EGFR signaling pathway. Patterns of drug response revealed unexpected common mechanisms. Future work will focus on informing patient care decisions with these results and determining if improvements in patient outcomes are realized. Citation Format: Shrey Patel, Sana Khalili, Victoria Moy, Emma Gray, Sawyer Lyons, Riley Brents, Carolyn Banister, Phillip J. Buckhaults. A multiplex organoid avatar drug testing platform for precision medicine [abstract]. In: Proceedings of the American Association for Cancer Research Annual Meeting 2023; Part 2 (Clinical Trials and Late-Breaking Research); 2023 Apr 14-19; Orlando, FL. Philadelphia (PA): AACR; Cancer Res 2023;83(8_Suppl):Abstract nr LB162.

Silicon Nanoparticle-Based Ratiometric Fluorescence Probes for Highly Sensitive and Visual Detection of VB2.

In this work, blue fluorescent silicon nanoparticles (SiNPs) were prepared by a simple one-step hydrothermal method using (3-aminopropyl) triethoxy silane (APTES) and eriochrome black T as raw materials. The SiNPs showed favorable water solubility, thermal stability, pH stability, salt tolerance, and photobleaching resistance. At an excitation wavelength of 376 nm, the SiNPs emitted bright blue fluorescence at 460 nm. In the presence of vitamin B2 (VB2), the fluorescence intensity (FL intensity) of the SiNPs at 460 nm decreased obviously, and a new peak appeared at 521 nm. Based on this, a novel ratiometric fluorescence method was established for VB2 detection. There was a good linear relationship between the fluorescence intensity ratio (F 521/F 460) and VB2 concentration from 0.5 to 60 μM with a detection limit of 135 nM. This method was successfully applied to detect VB2 content in the samples of vitamin B2 drugs and beverages. Additionally, a simple paper sensor based on the SiNPs was designed to visualize detection of VB2. With the support of color recognition software on a smartphone, the visual quantitative analysis of VB2 was realized, ranging from 40 to 800 μM.

Simultaneous quantitation of 17 female sex hormones in illegal products by validated LC-high resolution MS and LC-tandem MS methods.

The consumption of food and drugs adulterated with female sex hormones can have an extremely adverse effect on human health. Therefore, developing appropriate monitoring methods for the identification of various exogenous female sex hormones is crucial for minimizing and eliminating the related health risks. Herein, 17 female hormones categorized into two groups, estrogen and progestin, were analyzed using reversed phase LC coupled to Orbitrap or triple quadrupole MS. The fragmentation patterns for all compounds were discovered, and fragmented structures were also derived from them through LC-high resolution MS followed by qualitative sample analysis. In addition, quantitative analysis of 67 samples of illicit drugs and dietary supplements was performed using the validated LC-tandem MS method. Female hormone components were detected in two samples of an unauthorized injectable solution and a tablet-type drug. Medroxyprogesterone was detected in the samples in the range of 96.4-206 ng/g. Notably, eight components similar in structure to steroids were simultaneously detected as male sex hormones by confirming their fragmentation ion patterns using LC-high resolution MS. The developed methods thus offer a dependable, and practically applicable approach for the screening and detection of exogenous female sex hormones in real food and drug samples to ensure public health. This article is protected by copyright. All rights reserved.

The efficacy of complex solid dispersions of anthelmintics against experimental trichinellosis

The purpose of the research is to study the influence of various technological factors on obtaining of complex solid dispersions of anthelmintics with polyvinylpyrrolidone and licorice extract on anthelmintic efficacy in experimental trichinellosis of white mice.Materials and methods. The study of the nematodocidal activity of complex solid dispersions samples based on fenbendazole (FBZ), fenasal (FNS) and praziquantel (PZQ) with polyvinylpyrrolidone (PVP) and licorice extract (LE) obtained by mechanochemical technology at different ratios of components and different exposure times was carried out on 130 white mice experimentally infected with Trichinella spiralis in two experiments. On the 3rd day after infection, the animals were divided into experimental groups of 10 animals each. Samples of various complex solid dispersions of anthelmintics were administered intragastrically to the mice of the experimental groups at a dose of 2 mg/kg according to the active substance. FBZ substance was used as the basic drug at a dose of 2 mg/kg according to the active substance. Animals of the control groups did not receive the drugs. The animals were killed by decapitation on the 4th day after experimental drug samples administration, and the activity of the drugs was counted according to the results of helminthological necropsy of the intestine, the efficacy was calculated by the type of control test.Results and discussion. The efficacy of complex solid dispersions of FBZ and FNS with PVP polymer was higher in comparison with the activity of complexes with LE at the same duration of mechanochemical treatment in a roller mill. The FBZ activity decreased from 67.05 to 37.77% with a decrease in the duration of mechanochemical treatment from 24 h to 5 h and the efficacy of the FBZ : FNS complex with LE turned out to be almost at the level of the basic drug when treated for 1 h. The use of mechanochemical technology for obtaining of a solid dispersion of FBZ : FNS with PVP for targeted delivery makes it possible to increase the anthelmintic efficacy by 2.7 times compared with the activity of the FBZ substance, and with LE by 2.2 times. It was noted that complex solid dispersions of PBZ with PZQ have lower biological activity in comparison with compositions of FBZ with FNS.

Stability of Vancomycin and Ceftazidime With Prolonged Storage at -20°C.

Vancomycin and ceftazidime are commonly used intravitreal antibiotics for suspected bacterial endophthalmitis. Many retina surgical practices prepare aliquoted individual doses in syringes that are then stored frozen for future use, but this practice has not been well studied. This investigation aims to examine the stability of frozen vancomycin and ceftazidime. Samples of drugs were reconstituted monthly and placed in a -20°C freezer. At the end of 3 months and again at 6 months, a newly reconstituted drug constant was created and compared to a newly created reference sample. The frozen samples were compared to a freshly produced drug solution. Using high-performance liquid chromatography (HPLC), the peak heights were compared to evaluate stability. The vancomycin reference sample was 100 ± 1.67%. Values over time were 97.4 ± 0.75%, 98.8 ± 0.44%, 102.1 ± 0.4%, 100.5 ± 0.12%, 101.8 ± 0.12, 101.5 ± 0.11, and 100.6 ± 1.87 for 1, 2, 3(A), 3(B), 4, 5, and 6 months, respectively. The ceftazidime reference sample was 100 ± 1.8%. Values over time were 100.7 ± 1.78%, 100.0 ± 1%, 102.3 ± 1.55%, 117.5 ± 11.6%, 112.8 ± 1.64%, 123 ± 2.8%, and 117 ± 2.5% for 1, 2, 3(A), 3(B), 4, 5, and 6 months, respectively. Both vancomycin and ceftazidime were stable over 6 months under frozen conditions at -20°C. [Ophthalmic Surg Lasers Imaging Retina 2023;54:281-283.].

Substances from unregulated drug markets - A retrospective data analysis of customer-provided samples from a decade of drug checking service in Zurich (Switzerland).

Drug checking services (DCS) are harm reduction interventions for people who consume illicit substances. Unregulated drug markets lead to samples with unexpected and variable contents. A retrospective data analysis of Zurich's DCS was performed to determine the nature of these samples. This study aims to investigate the qualitative and quantitative properties of 16,815 customer-provided psychoactive drug samples analyzed chemically through the DCS in Zurich from 1st January 2011 to 31st December 2021. The main analytical method utilized for characterizing these substances was high-performanceliquid chromatography and gas chromatography-mass spectrometry. Data sets are summarized using descriptive statistics. There was a 2.5-fold increase in the number of tested samples over the past decade. An overall proportion of 57.9% (weighted mean) of samples within our database demonstrates unexpected analytical findings and additional low sample contents during the observation period. Substantial differences in quality and quantity between substance groups were detected and an increase of sample quality and content over time was demonstrated. Chemical analysis reveals that over half of substances acquired from unregulated drug markets analyzed through DCS in Zurich are with low qualitative and quantitative properties, which may expose users to risks. Based on longitudinal analyses over a decade, this study contributes to the body of evidence that DCS may potentially manipulate unregulated drug markets towards providing better quality substances, as well as may stabilize these markets over time. The necessity for drug policy changes to make this service accessible in further settings was highlighted, as DCS still often take place in legal grey zones. None to declare.

Application of ISO 17025 Standards in the Validation of a Spectrophotometric Method for Quality Assessment of Generic Brands of Cetirizine Tablets marketed in Nigeria.

Background: The concern for the quality of medicines is to ensure effiffifficacious clinical outcomes and quality health care. The World Health Organization (WHO) estimates that 10–20 % of medicines in developing country markets are sub-standard. Continuous  monitoring of the quality of medicines requires both competent analysts and well-equipped drug quality control laboratories with  international accreditation. The objective of the study was to evaluate the quality control parameters of the generic cetirizine  dihydrochloride 10 mg tablets marketed in Abuja metropolis of Nigeria and to validate and apply a UV spectrophotometric method to  the assay of the commercial tablet formulations.  Method: Nine brands of cetirizine dihydrochloride tablets were randomly selected from retail pharmacy stores and quality control  tests of weight variation, friability, hardness, disintegration, and dissolution parameters were conducted per United States  Pharmacopoeia (USP) standards. Thickness and diameter were also evaluated by standard methods. AUVspectrophotometric method  was adopted and validated according to ICH guidelines and applied for the drug assay of the tablet dosage units.  Results: The  thickness, diameter, hardness and disintegration tests for the drug samples ranged from 2.81–3.76 mm, 3.88–8.11 mm  1.65–7.50 KgF and 0.44–4.90 min, respectively. All the samples met the compendial specififications for the weight variation test and also  for the friability and dissolution tests which ranged 0.18–0.56 % and 90.15–109.18 % at 30 min, respectively. The studies for  validation of the UV method demonstrated good linearity with a correlation coeffiffifficient of r2 = 0.9989 in the concentration range of  2.5–25 µg/mL of cetirizine dihydrochloride (CTZ) reference standard and the limit of detection (LOD) and limit of quantitation (LOQ)  were 0.42 µg/mL and 1.29 µg/mL, respectively. The % RSD of the precision studies was less than the 2 % standard limit and the  accuracy (recovery) ranged from 100.9‒103.4 %. The percentage contents of the generic brands were determined and ranged from  99.12–103.21 % and were within the offiffifficial specififications.  Conclusion: The UV method was simple, sensitive and rapid and  successfully applied to the assay of nine commercial brands of CTZ  tablets. All the drugs met the compendial specififications on the quality parameters. &nbsp

Validated portable device for the qualitative and quantitative electrochemical detection of MDMA ready for on-site use

Identifying and quantifying 3,4-methyl​enedioxy​methamphetamine (MDMA) on-site in suspected illicit drug samples, whether it be at recreational settings or manufacturing sites, is a major challenge for law enforcement agencies (LEAs). Various analytical techniques exist to fulfil this goal, e.g. colourimetry and portable spectroscopic techniques, each having its specific limitations (e.g. low accuracy, fluorescence, no quantification) and strengths (e.g. fast, easy to use). In this work, for the first time, an electrochemical MDMA sensor is presented to become a detection tool that can realistically be used on-site. More specifically, the use of a single buffer solution and an unmodified screen-printed electrode, along with the integration of a data analysis algorithm and mobile application permits the straightforward on-site identification and quantification of MDMA in suspicious samples. Multiple studies investigating different parameters, including pH, concentration, reproducibility, temperature and binary mixture analyses, were executed. To fully understand all the occurring redox processes, liquid chromatography coupled with high-resolution mass spectrometry analysis of partially electrolyzed MDMA samples was performed unravelling oxidation of the methylenedioxy group. Validation of the methodology was executed on 15 MDMA street samples analysed by gas chromatography coupled with mass spectrometry and compared with the performance of a commercial portable Raman and Attenuated Total Reflection Fourier Transform Infrared Spectroscopy (ATR-FTIR) device. The novel methodology outperformed the spectroscopic techniques, correctly identifying all 15 street samples. Additionally, the electrochemical sensor predicted the purity of the tablets with a mean absolute error of 2.3%. Overall, this new, electrochemical detection strategy provides LEAs the rapid, low-cost, on-site detection and quantification of MDMA in suspicious samples, without requiring specialized training.

Simple Sensor Application: Determination of Electrochemical Properties of Carvedilol in CPE Based on Zinc Oxide Nanoparticles and Development of the Method for its Determination in Pharmaceutical Samples

In the study, the electrochemical characteristics of carvedilol were determined by cyclic voltammetry and square wave voltammetry on carbon paste electrode with zinc oxide nanoparticles at pH 8.0 in Britton Robinson buffer. The adsorption characteristics of the molecule on the modified electrode and the electron number accompanying the electrode reaction were calculated. In addition, a new square wave anodic adsorptive stripping voltammetry process was suggested for the determination of carvedilol drug samples. The linear concentration range and detection limit of the process were found to be 0.07 µM–2.61 µM and 0.09 µM, respectively. Recovery studies of CAR in the pharmaceutical sample were performed to check the accuracy of the developed process. With the developed process, results with high reliability, reproduceability, accuracy and precision were obtained for the determination of CAR in pharmaceutical samples.

Synthesis and Characterization of Magnetic Molecularly Imprinted Polymer for the Monitoring of Amoxicillin in Real Samples Using the Chromatographic Method

Amoxicillin (AMX) is an antibiotic frequently used for the treatment of bacterial disorders and respiratory problems in both humans and animals. This work aims to synthesize a molecularly imprinted superparamagnetic polymer (SP-MIP) with a core-shell structure for the selective detection of AMX in real samples. Magnetite superparamagnetic nanoparticles (SNP) were prepared by the polyol method, coated with silica, and functionalized with silane groups. The polymerization process was executed using the free-radical precipitation method. Thermogravimetric analysis (TGA) was used to evaluate the thermal stability of the synthesized materials. The results obtained from N2 adsorption and desorption analyses showed that the surface area of SP-MIP (19.8 m2/g) was higher than that of the non-molecularly imprinted superparamagnetic polymer (SP-NIP—9.24 m2/g). The optimized adsorption analysis showed that both SP-MIP and SP-NIP followed SIP-type behavior, with adsorption constant KS 0.01176, 1/n 1.73. The selectivity tests showed that SP-MIP is highly selective for AMX in the presence of other molecules. Finally, for the recovery analysis, the application of SP-MIP for determining AMX in samples of tap water, river water, and drugs using HPLC yielded a mean recovery value of 94.3%.

Development of qualitative GC MS method for simultaneous identification of PM-CCM a modified illicit drugs preparation and its modern-day application in drug-facilitated crimes

Prescriptions for psychoactive substances such as Pregabalin, Methamphetamine, Caffeine, Clonazepam and Mirtazapine (PM-CCM) are common in the treatment of a variety of disorders. Indeed, the PM-CCM has been used in different therapeutic areas, including insomnia, anxiety, seizure disorders, etc. Unfortunately, these psychoactive substances are present in the illegal street market, leading to a lot of drug abuse among some addicted users, road insecurity and suicide. Hence, it has become essential to validate and develop a rapid and effective method to analyze the PM-CCM, a modified illicit drug, for drug abuse in the forensic sciences. A simple, rapid, specific and sensitive Gas Chromatography-Mass Spectrometry(GC-MS) method has been developed for the identification of Pregabalin, Methamphetamine, Caffeine, Clonazepam and Mirtazapine (PM-CCM) in forensic exhibits. At room temperature, the sample was ultrasonicated for 5 minutes before being extracted with methanol. A highly precise auto-injector is used to inject a very small quantity of samples for analysis. Helium is used as a carrier gas with a flow rate of 1 ml/min. The separation of PM-CCM was performed on SH-RXi-5 MS, ID.25 mm, film thickness. 25 µm, length of 30 m column. The constituents of PM-CCM were identified by the mass-to-charge ratio (m/z ratio) of fragments of the parent compound by comparing them with the NIST-17 MS Library. Separation and identification of PM-CCM were achieved within a 15-minute run. The proposed method has been successfully used for the routine analysis of PM-CCM in complex illicit drug preparations and in forensic exhibits as well. The application of above discussed qualitative analysis method and screening of PM-CCM, modified illicit drug samples demonstrates the potential and applicability of the technique to the fast chemical profiling of illicit samples.