Comprehensive analysis of vitamin D impurities in oily drug products using supercritical fluid chromatography-mass spectrometry.

Vitamin D, an essential micronutrient, often requires supplementation via medicines or food supplements, which necessitate quality control (QC). This study presents the development of a method for detecting and quantifying seven impurities of vitamin D in oily drug products using supercritical fluid chromatography-mass spectrometry (SFC-MS). Targeted impurities include two esters of vitamin D and five non-esters including four that are isobaric to vitamin D.

Emerging analytical techniques for pharmaceutical quality control: Where are we in 2022?

Quality control is a fundamental and critical activity in the pharmaceutical industry that guarantees the quality of medicines. QC analyses are currently performed using several well-known techniques, mainly liquid and gas chromatography. However, current trends are focused on the development of new techniques to reduce analysis time and cost, to improve the performances and decrease ecological footprint.

Critical review on recent trends in cannabinoid determination on cannabis herbal samples: From chromatographic to vibrational spectroscopic techniques.

Cannabis has been at the center of scientific attention for some years now. Since its pharmacological potential has been highlighted, cannabis has become a hot topic in research laboratories, leading to the publication of many scientific studies. Focusing on analytical chemistry, an enormous number of analytical methods for cannabinoid (CNB) determination have been published, involving various techniques.

Selection of essential spectra to improve the multivariate curve resolution of minor compounds in complex pharmaceutical formulations.

Multivariate curve resolution unmixing of hyperspectral imaging data can be challenging when low sources of variance are present in complex samples, as for minor (low-concentrated) chemical compounds in pharmaceutical formulations. In this work, it was shown how the reduction of hyperspectral imaging data matrices through the selection of essential spectra can be crucial for the analysis of complex unknown pharmaceutical formulation applying Multivariate Curve Resolution - Alternating Least Squares (MCR-ALS). Results were obtained on simulated datasets and on real FT-IR and Raman hyperspectral images of both genuine and falsified tablets.

Generic SFC-MS methodology for the quality control of vitamin D oily formulations.

Vitamin D is a key micronutrient whose intakes are inadequate for most populations worldwide. Supplementation with medicines or food supplements is commonly prescribed to correct this imbalance and the quality of these products must be ensured. In this context, a generic methodology for the assay of vitamin D in oily formulations is proposed using supercritical fluid chromatography coupled to mass spectrometry (SFC-MS).

Optimization of a robust and reliable FITC labeling process for CE-LIF analysis of pharmaceutical compounds using design of experiments strategy.

Fluorescence, especially laser induced fluorescence (LIF), is a powerful detection technique thanks to its specificity and high sensitivity. The use of fluorescence detection hyphenated to separation technique often requires the labeling of analytes with suitable fluorescent dye, such as FITC for the labeling of molecules presenting amino groups. Nevertheless, the labeling of analytes could be a tedious, time consuming and a non-robust step of the analytical workflow.

Interlaboratory study of a supercritical fluid chromatography method for the determination of pharmaceutical impurities: Evaluation of multi-systems reproducibility.

Modern supercritical fluid chromatography (SFC) is now a well-established technique, especially in the field of pharmaceutical analysis. We recently demonstrated the transferability and the reproducibility of a SFC-UV method for pharmaceutical impurities by means of an inter-laboratory study. However, as this study involved only one brand of SFC instrumentation (Waters®), the present study extends the purpose to multi-instrumentation evaluation.

Pixel-based Raman hyperspectral identification of complex pharmaceutical formulations.

Hyperspectral imaging has been widely used for different kinds of applications and many chemometric tools have been developed to help identifying chemical compounds. However, most of those tools rely on factorial decomposition techniques that can be challenging for large data sets and/or in the presence of minor compounds. The present study proposes a pixel-based identification (PBI) approach that allows readily identifying spectral signatures in Raman hyperspectral imaging data.

Development of a sensitive MEKC-LIF method for synthetic cathinones analysis.

Synthetic cathinones are phenylalkylamine compounds related to natural cathinone from Catha edulis leaves. Due to their sympathomimetic effects comparable to common illicit drugs, these substances are mainly drugs of abuse and constitute the second most frequently seized group of new psychoactive substances. In order to ensure their regulation and to promote public health, reliable analytical tools are required to track these substances.

The analysis of cannabinoids in cannabis samples by supercritical fluid chromatography and ultra-high-performance liquid chromatography: A comparison study.

The aim of this work was to develop a supercritical fluid chromatographic method to study the applicability of this emerging technique to cannabinoid analysis and showcase its advantages. During method development, the authors focused on nine phyto-cannabinoids to assess the selectivity needed to potentially perform the quantitation of each cannabinoid. After method development, robustness studies were carried out on this method to gain more information about its qualitative behavior (in terms of critical resolutions) when varying some crucial parameters (concentration of additive, column temperature, starting gradient conditions and column batch).

Evaluation of the analytical performances of two Raman handheld spectrophotometers for pharmaceutical solid dosage form quantitation.

This paper addresses the issue of pharmaceutical solid dosage form quantitation using handheld Raman spectrophotometers. The two spectrophotometers used are designed with different technologies: one allows getting a more representative sampling with the Orbital Raster Scanning technology and the other one allows setting acquisition parameters. The goal was to evaluate which technology could provide the best analytical results.

Comparison of hyperspectral imaging techniques for the elucidation of falsified medicines composition.

Hyperspectral imaging has shown a high potential to analyze falsifications of solid pharmaceutical products since the last decade. Thanks to the non-destructive, ecological and non-invasive properties, it is a preferred technique for these kinds of applications. Moreover, thanks to the spectroscopic properties, it is possible to detect as well organic compounds as inorganic compounds in a single analysis.

Implementation of a generic SFC-MS method for the quality control of potentially counterfeited medicinal cannabis with synthetic cannabinoids.

In this study, we describe the development of a SFC-MS method for the quality control of cannabis plants that could be potentially adulterated with synthetic cannabinoids. Considering the high number of already available synthetic cannabinoids and the high rate of development of novel structures, we aimed to develop a generic method suitable for the analysis of a large panel of substances using seventeen synthetic cannabinoids from multiple classes as model compounds. Firstly, a suitable column was chosen after a screening phase.

Supercritical fluid chromatography: a promising alternative to current bioanalytical techniques.

During the last years, chemistry was involved in the worldwide effort toward environmental problems leading to the birth of green chemistry. In this context, green analytical tools were developed as modern Supercritical Fluid Chromatography in the field of separative techniques. This chromatographic technique knew resurgence a few years ago, thanks to its high efficiency, fastness and robustness of new generation equipment.

Combination of partial least squares regression and design of experiments to model the retention of pharmaceutical compounds in supercritical fluid chromatography.

This work presents a first attempt to establish a model of the retention behaviour for pharmaceutical compounds in gradient mode SFC. For this purpose, multivariate statistics were applied on the basis of data gathered with the Design of Experiment (DoE) methodology. It permitted to build optimally the experiments needed, and served as a basis for providing relevant physicochemical interpretation of the effects observed.

Quantitative determination of salbutamol sulfate impurities using achiral supercritical fluid chromatography.

In the last years, supercritical fluid chromatography has largely been acknowledged as a singular and performing technique in the field of separation sciences. Recent studies highlighted the interest of SFC for the quality control of pharmaceuticals, especially in the case of the determination of the active pharmaceutical ingredient (API). Nevertheless, quality control requires also the determination of impurities.

Screening study of SFC critical method parameters for the determination of pharmaceutical compounds.

Nowadays, supercritical fluid chromatography is commonly presented as a promising alternative technique in the field of separation sciences. Nevertheless the selection of chromatographic conditions and sample preparation of pharmaceutical compounds remain a challenge and peak distortion was previously highlighted. The main objective of the present work was to evaluate the impact of different critical method parameters (CMPs), i.

Evaluation of the quantitative performances of supercritical fluid chromatography: from method development to validation.

Recently, the number of papers about SFC increased drastically but scientists did not truly focus their work on quantitative performances of this technique. In order to prove the potential of UHPSFC, the present work discussed about the different steps of the analytical life cycle of a method: from development to validation and application. Moreover, the UHPSFC quantitative performances were evaluated in comparison with UHPLC, which is the main technique used for quality control in the pharmaceutical industry and then could be considered as a reference.

Robust method optimization strategy-a useful tool for method transfer: the case of SFC.

The concept of Quality by Design (QbD) is now well established in pharmaceutical industry and should be applied to the development of any analytical methods. In this context, the key concept of Design Space (DS) was introduced in the field of analytical method optimization. In chromatographic words, the DS is the space of chromatographic conditions that will ensure the quality of peaks separation, thus DS is a zone of robustness.

Innovative green supercritical fluid chromatography development for the determination of polar compounds.

In the context of green analytical chemistry, a supercritical fluid chromatography method was developed. In order to prove the potential of this technology, a worst case was selected, i.e.