A validated ultra-performance liquid chromatography with diode array detection coupled to electrospray ionization and triple quadrupole mass spectrometry method to simultaneously quantify taurine, homotaurine, hypotaurine and amino acids in macro- and microalgae

A fast and reliable method for the simultaneous quantification of Taurine, Homotaurine, Hypotaurine and 19 amino acids in algae samples by Ultra-performance liquid chromatography coupled with diode array and tandem mass spectrometry (UHPLC–DAD-MS/MS) was optimized and validated. Target compounds were chromatographically resolved in less than 15 min. (ESI)-MS/MS electrospray ionization and pure analytical standards were used to confirm the identity of all analytes, while quantitation was carried out with diode array detection. Validation parameters of the method were satisfactory: Resolution of peak pairs was always higher than 1.55; all analytical curves showed R2 > 0.99, with working ranges between 0.04 mg/g to 33.1 mg/g and 9.13 mg/g to 107 mg/g and the Lack-of-fit test was not significant. The intra and inter-day precision of the method (expressed as relative standard deviation) were lower than 6% and recovery values ranged between 95% and 105%. The method was demonstrated to be robust to small deliberate variations of seven variables such sample weight, volume of hydrolysis reagent, hydrolysis time and temperature, derivatization time, column temperature and flow rate. The mean expanded uncertainty for all the target compounds were 0.7 mg/g with a coverage factor of 2. Method Limits of detection and quantification varied from 0.005 * 10−3 mg/g to 0.11 * 10−3 mg/g and 0.01* 10−3 mg/g to 0.22 * 10-3 mg/g respectively, allowing the routine determination of these bioactive compounds in algae extracts. Therefore, the method was successfully applied for the quantitative determination of the 22 target compounds in five seaweed commercial samples. Relevant compounds were quantified for the first time in the five algae species, namely: i) Taurine in Gracilaria longissima and Chlorella spp., ii) Gamma-aminobutyric acid in G. longissima and L. japonica, iii) Hydroxyproline in G. longissima, Ulva lactuca, Porphyra spp., and L. japonica and iv) Homotaurine and Hypotaurine in the five species studied.info:eu-repo/semantics/acceptedVersio

3D inkjet printing of tablets exploiting bespoke complex geometries for controlled and tuneable drug release

A hot melt 3D inkjet printing method with the potential to manufacture formulations in complex and adaptable geometries for the controlled loading and release of medicines is presented. This first use of a precisely controlled solvent free inkjet printing to produce drug loaded solid dosage forms is demonstrated using a naturally derived FDA approved material (beeswax) as the drug carrier and fenofibrate as the drug. Tablets with bespoke geometries (honeycomb architecture) were fabricated. The honeycomb architecture was modified by control of the honeycomb cell size, and hence surface area to enable control of drug release profiles without the need to alter the formulation. Analysis of the formed tablets showed the drug to be evenly distributed within the beeswax at the bulk scale with evidence of some localization at the micron scale. An analytical model utilizing a Fickian description of diffusion was developed to allow the prediction of drug release. A comparison of experimental and predicted drug release data revealed that in addition to surface area, other factors such as the cell diameter in the case of the honeycomb geometry and material wettability must be considered in practical dosage form design. This information when combined with the range of achievable geometries could allow the bespoke production of optimized personalised medicines for a variety of delivery vehicles in addition to tablets, such as medical devices for example

In silico toxicology protocols

The present publication surveys several applications of in silico (i.e., computational) toxicology approaches across different industries and institutions. It highlights the need to develop standardized protocols when conducting toxicity-related predictions. This contribution articulates the information needed for protocols to support in silico predictions for major toxicological endpoints of concern (e.g., genetic toxicity, carcinogenicity, acute toxicity, reproductive toxicity, developmental toxicity) across several industries and regulatory bodies. Such novel in silico toxicology (IST) protocols, when fully developed and implemented, will ensure in silico toxicological assessments are performed and evaluated in a consistent, reproducible, and well-documented manner across industries and regulatory bodies to support wider uptake and acceptance of the approaches. The development of IST protocols is an initiative developed through a collaboration among an international consortium to reflect the state-of-the-art in in silico toxicology for hazard identification and characterization. A general outline for describing the development of such protocols is included and it is based on in silico predictions and/or available experimental data for a defined series of relevant toxicological effects or mechanisms. The publication presents a novel approach for determining the reliability of in silico predictions alongside experimental data. In addition, we discuss how to determine the level of confidence in the assessment based on the relevance and reliability of the information