Derivatization Method Research Articles

Comparison of Derivatization Methods for Groomed Latent Print Residues Analysis via Gas Chromatography

The practice of latent print analysis is comprised of a visual examination and the comparison of the fingerprint pattern from a questioned print to an exemplar(s). When a questioned print is either smudged or contains little pattern detail, the print comparison would be considered an inconclusive determination. However, in these scenarios, the latent print residues (LPRs) could provide associative information to supplement the current ACE-V (Analysis, Comparison, Examination-Verification) process. Advancements using analytical techniques allow for the analysis of LPR chemistry; however, derivatization is generally required to increase the abundance of components not traditionally observed in gas chromatography. This study aimed to determine whether two derivatization reagents, boron trifluoride in methanol (BF3-MeOH) and N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA), provide a better recovery of LPR components from a porous or non-porous substrate. Five volunteers deposited groomed latent print samples onto two substrates: a microfiber filter (porous) and a microscope slide (non-porous). The residues were derivatized or evaporated prior to the gas chromatography-mass spectrometry (GC-MS) analysis. The percent recoveries were higher, >83%, in the DCM extracted samples for both substrates compared to those samples prepared in hexanes. DCM/MSTFA derivatization provided the recovery of fatty acids that ranged from 20 to 30% for both substrates and a recovery of squalene at a rate of 2.37% for the filter sample and 4.2% for the slide sample. These rates were higher than the recovery rates obtained for the hexanes/BF3-MeOH-derivatized samples, with a range of 1–8% for the fatty acids recovery rates and 0.6–0.85% for squalene from both substrates. Overall, the MSTFA derivatization reagent produced higher recoveries for LPR on porous and non-porous substrates while providing a LPR chromatographic profile similar to that of a non-derivatized sample. The use of DCM as a solvent provided a wider range of LPR components recovered than hexanes and, thus, should be used as the extraction solvent when derivatizing samples, regardless of the substrate.

A novel strategy on the study of whole intestinal metabolic profiles for Polygalae Radix before and after processing.

Relieving toxicity and enhancing a calming effect after processing Polygalae Radix (PR) are widely known. Aromatic carboxylic acids (ACAs) may be crucial processed products. However, due to the limited detection methods for ACAs, the whole metabolic profiles via intestinal bacteria are still not very clear. Designing a novel strategy for the detection of ACAs and tracking the whole metabolic profiles before and after processing PR. The stable-isotope labelling derivatisation (SILD) method based on multidimensional ultra-high performance liquid chromatography coupled with a mass spectrometer (UHPLC-MS) technology and UNIFI-pathway mode was firstly designed to systematically study the metabolisms of all the drug-derived ingredients ranging from m/z 100 to 2000 in processing PR via intestinal bacteria. Firstly, the SILD with UHPLC coupled with a triple-quadrupole MS technology was designed to trace eight ACA metabolites of the processed PR with intestinal bacteria. Additionally, the UHPLC coupled with a quadrupole time-of-flight MS with UNIFI-pathway mode was adopted to monitor relatively big metabolites. The metabolism mechanism of ACAs (eight kinds) and the relatively big molecular metabolites (98 kinds) were deeply traced in PR, PR with refined honey (HP), and PR with licorice (LP) via the intestinal bacteria. Totally 106 intact metabolic profiles of drug-derived ingredients were presented. Importantly, the influence of LP on the metabolism of compounds after incubation of intestinal bacteria was greater than that of HP. This research provides a comprehensive and systematic guidance for further study on in vivo metabolisms of the processed PR.

A novel reagent pre-column derivatization method for UHPLC-MS/MS to determine four α-dicarbonyl compounds in beer

A novel reagent pre-column derivatization method for UHPLC-MS/MS to determine four α-dicarbonyl compounds in beer

A Rapid Derivatization for Quantitation of Perfluorinated Carboxylic Acids from Aqueous Matrices by Gas Chromatography-Mass Spectrometry.

Ultrashort-chain perfluorinated carboxylic acids (PFCAs) are receiving more attention due to their ever-increasing presence in the environment. Methods have been established for the analysis of short- and long-chain PFCAs, while robust quantitation of ultrashort-chain species is scarce. Here, we develop a novel derivatization method using diphenyl diazomethane for quantitation of C2-C14 PFCAs in aqueous matrices. The method is highlighted by rapid completion of derivatization (<1 min) and retention and separation of ultrashort-chain (C2/C3) PFCA derivatives using H2 carrier gas (R > 1.5). A weak anion exchange solid-phase extraction procedure for analyte recovery from representative aqueous samples was developed and validated by spike and recovery from ultrapure water, synthetic ocean water, and simulated denuder extracts used for collecting gaseous PFCAs. Recoveries for PFCAs ranged from 83 to 130% for the majority of analytes and matrices. The instrument detection limits (IDLs) range from 8 to 220 fg per injection, and method detection limits (MDLs) range from 0.06 to 14.6 pg/mL for 500 mL aqueous samples, which are within an order of magnitude to conventional LC-MS/MS methods. The method was applied to the analysis of real samples of tap water, rainwater, ocean water, and annular denuder extracts. The overall method provides a cost-effective alternative to conventional LC-MS/MS methods, overcoming the typical GC-MS drawbacks of high detection limits and long sample preparation times while being able to simultaneously analyze the complete spectrum of environmentally relevant PFCAs.

On-tissue chemical derivatization of volatile metabolites for matrix-assisted laser desorption/ionization mass spectrometry imaging.

Mass spectrometry imaging (MSI) of volatile metabolites is challenging, especially in matrix-assisted laser desorption/ionization (MALDI). Most MALDI ion sources operate in vacuum, which leads to the vaporization of volatile metabolites during analysis. In addition, tissue samples are often dried during sample preparation, leading to the loss of volatile metabolites even for other MSI techniques. On-tissue chemical derivatization can dramatically reduce the volatility of analytes. Herein, a derivatization method is proposed utilizing N,N,N-trimethyl-2-(piperazin-1-yl)ethan-1-aminium iodide to chemically modify short-chain fatty acids in chicken cecum, ileum, and jejunum tissue sections before sample preparation for MSI visualization.

Dissipation Dynamic, Residue Distribution and Risk Assessment of Emamectin Benzoate in Longan by High-Performance Liquid Chromatography with Fluorescence Detection.

A derivatization method combined with high-performance liquid chromatography-fluorescence detection (HPLC-FLD) was used to evaluate the dissipation, residue distribution and risk assessment of emamectin benzoate in whole longan and pulp. The average recoveries were 82-111% with relative standard deviation (RSD) less than 11%. The limit of quantification (LOQ) was 0.001 mg/kg in longan and pulp. The half-lives were 3.3-4.2 days. The terminal residues in whole longan were <0.001-0.025 mg/kg applied two and three times at two levels of dosage with PHIs of 10, 14, and 21 days. The residues in whole longan had a higher quantity than those in the pulp, and the terminal residues of pulp were all lower than LOQ (0.001 mg/kg). The chronic risk of emamectin benzoate was not negligible to humans depending on ADI% value, which was higher than 1; and the acute risk was acceptable to the consumer. This study could provide guidance for the safe use of emamectin benzoate in longan and serve as a reference for the establishment of maximum residue limits (MRLs) in China.

In situ droplet-based on-tissue chemical derivatization for lipid isomer characterization using LESA.

In this work, we present an in situ droplet-based derivatization method for fast tissue lipid profiling at multiple isomer levels. On-tissue derivatization for isomer characterization was achieved in a droplet delivered by the TriVersa NanoMate LESA pipette. The derivatized lipids were then extracted and analyzed by the automated chip-based liquid extraction surface analysis (LESA) mass spectrometry (MS) followed by tandem MS to produce diagnostic fragment ions to reveal the lipid isomer structures. Three reactions, i.e., mCPBA epoxidation, photocycloaddition catalyzed by the photocatalyst Ir[dF(CF3)ppy]2(dtbbpy)PF6, and Mn(II) lipid adduction, were applied using the droplet-based derivatization to provide lipid characterization at carbon-carbon double-bond positional isomer and sn-positional isomer levels. Relative quantitation of both types of lipid isomers was also achieved based on diagnostic ion intensities. This method provides the flexibility of performing multiple derivatizations at different spots in the same functional region of an organ for orthogonal lipid isomer analysis using a single tissue slide. Lipid isomers were profiled in the cortex, cerebellum, thalamus, hippocampus, and midbrain of the mouse brain and 24 double-bond positional isomers and 16 sn-positional isomers showed various distributions in those regions. This droplet-based derivatization of tissue lipids allows fast profiling of multi-level isomer identification and quantitation and has great potential in tissue lipid studies requiring rapid sample-to-result turnovers.

Photocatalytic reactive liquid microjunction surface sampling-mass spectrometry for rapid and selective in-situ analysis of alpha-unsubstituted amine metabolites or drugs in brain tissue

In in-situ mass spectrometry (MS), different on-tissue derivatization methods have been developed to enhance the signals of poorly ionizable primary amines. However, those chemical derivatization methods are laborious and time-consuming, and are usually limited to detection of high-abundance amino acids which suppress the reaction of low-abundance monoamine neurotransmitters and drugs. Herein, A rapid and selective photocatalytic derivatization technique for alpha-unsubstituted primary amine was developed with 5-hydroxyindole as derivatization reagent and TiO2 as photocatalyst, and was introduced into liquid microjunction surface sampling (LMJSS)-MS system as online derivatization. The results showed that the photocatalytic derivatization method largely enhanced the signals of primary amines by 5–300 fold, and were selective to alpha-unsubstituted primary amines. Thus, the suppression effects from high-abundance amino acids to the reaction of monoamine neurotransmitters and benzylamine drugs proved to be largely reduced in the new method (matrix effect>50%) comparing with those in chemical derivatization method (matrix effect<10%). In addition, the optimal pH of the derivatization reaction was measured to be 7, which indicates the mild and physiologically compatible reaction conditions. By in-situ synthesis of TiO2 monolith in the transfer capillary of the LMJSS-MS system, rapid on-line photocatalytic derivatization was achieved and completed in 5 s during the transfer of sampling extract from the flow-probe to the MS inlet. With the new photocatalytic reactive LMJSS-MS method, detection limits of three primary amines on glass slides were in the range of 0.031–0.17 ng/mm2 with acceptable linearity (r=0.9815–0.9998) and relatively high repeatability (relative standard deviations <22.1%). Finally, endogenous tyramine, serotonin, two dipeptides and one doped benzylamine drug were identified and in-situ analyzed in the mouse cerebrum by the new method with largely enhanced signals comparing with LMJSS-MS without online derivatization. The new method provides a more selective, rapid and automated way to analyze alpha-unsubstituted amine metabolites and drugs in-situ comparing with traditional methods.

LC-MS/(MS) confirmatory doping control analysis of intact phase II metabolites of methenolone and mesterolone after Girard's Reagent T derivatization.

In the present study, the application and evaluation of Girard's Reagent T (GRT) derivatization for the simultaneous detection and significantly important identification of different phase II methenolone and mesterolone metabolites by LC-MS/(MS) are presented. For the LC-MS analysis of target analytes two complementary isolation methods were developed; a derivatization and shoot method in which native urine is diluted with derivatization reagent and is injected directly to LC-MS and a liquid-liquid extraction method, using ethyl acetate at pH 4.5, for the effective isolation of both sulfate and glucuronide metabolites of the named steroids as well as of their free counterparts. For the evaluation of the proposed protocols, urine samples from methenolone and mesterolone excretion studies were analyzed against at least one sample from a different excretion study. Retention times, along with product ion ratios, were evaluated according to the WADA TD2021IDCR requirements, in order to determine maximum detection and identification time windows for each metabolite. Established identification windows obtained after LC-MS/(MS) analysis were further compared with those obtained after GC-MS/(MS) analysis of the same samples from the same excretion studies, for the most common analytes monitored by GC-MS/(MS). Full validation was performed for the developed derivatization and shoot method for the identification of methenolone metabolite, 3α-hydroxy-1-methylen-5α-androstan-17-one-3-glucuronide (mth3). Overall, the GRT derivatization presented herein offers a tool for the simultaneous sensitive detection of free, intact glucuronide and sulfate metabolites by LC-MS/(MS) that enhance significantly the detection and identification time windows of specific methenolone and mesterolone metabolites for doping control analysis.

4H‐Pyrido[1,2‐a]pyrimidin‐4‐one, biologically important fused heterocyclic scaffold: Synthesis and functionalization

Abstract4H‐pyrido[1,2‐a]pyrimidin‐4‐one and their derivatives are highly bioactive and multipurpose heterocyclic motifs, having application in drugs, natural products, agrochemical, material science, and organic synthesis. The C‐H functionalization of basic core structure of heterocycles have become indispensable tools that have continually increased the importance in the pharmaceutical industry for the synthesis of various useful heterocyclic molecules and their derivatives. In this review, we have provided a summary of various routes to synthesize 4H‐pyrido[1,2‐a]pyrimidin‐4‐one derivatives along with various derivatization methods such as via cross‐coupling, C‐H functionalization through arylation, alkenylation, sulfenylation, selenylation, phosphonation etc. taking into account the synthetic potentiality and significant influence of this scaffold in drug discovery.

Three New Selaginellin Derivatives from Selaginella pulvinata and Their α-Glucosidase Inhibitory Activity.

Three new selaginellin derivatives, selaginpulvilins V-X (1-3), together with seven known analogs (4-10) were isolated from whole plants of Selaginella pulvinata. Their structures were determined by extensive spectroscopic methods including 1D and 2D NMR, HR-ESI-MS and chemical derivatization method. Compound 1 represents a rare example of naturally occurring selaginellin with an alkynylphenol-trimmed skeleton. Biological evaluation showed that compounds 2, 6 and 8 displayed moderate inhibition against α-glucosidase with IC50 values of 3.71, 2.04 and 4.00 μM, respectively.

A Novel Method for the Pre-Column Derivatization of Saccharides from Polygonatum cyrtonema Hua. by Integrating Lambert–Beer Law and Response Surface Methodology

Traditional Chinese medicine (TCM) safety and effectiveness can be ensured by establishing a suitable quality assessment system. This work aims to develop a pre-column derivatization HPLC method for Polygonatum cyrtonema Hua. quality control. In this study, 1-(4'-cyanophenyl)-3-methyl-5-pyrazolone (CPMP) was synthesized and reacted with monosaccharides derived from P. cyrtonema polysaccharides (PCPs), followed by HPLC separation. According to the Lambert-Beer law, CPMP has the highest molar extinction coefficient of all synthetic chemosensors. A satisfactory separation effect was obtained under a detection wavelength of 278 nm using a carbon-8 column and gradient elution over 14 min, with a flow rate of 1 mL per minute. Glucose (Glc), galactose (Gal), and mannose (Man) make up the majority of the monosaccharide components in PCPs, and their molar ratios are 1.73:0.58:1. The confirmed HPLC method has outstanding precision and accuracy, establishing a quality control method for PCPs. Additionally, the CPMP showed a visual improvement from colorless to orange after the detection of reducing sugars, allowing for further visual analysis.

Formation of carbonyl compounds during ozonation of lake water and wastewater: Development of a non-target screening method and quantification of target compounds

Ozonation of natural waters is typically associated with the formation of carbonyl compounds (aldehydes, ketones and ketoacids), a main class of organic disinfection byproducts (DBPs). However, the detection of carbonyl compounds in water and wastewater is challenged by multiple difficulties inherent to their physicochemical properties. A non-target screening method involving the derivatisation of carbonyl compounds with p-toluenesulfonylhydrazine (TSH) followed by their analysis using liquid chromatography coupled to electrospray ionisation high-resolution mass spectrometry (LC-ESI-HRMS) and an advanced non-target screening and data processing workflow was developed. The workflow was applied to investigate the formation of carbonyl compounds during ozonation of different water types including lake water, aqueous solutions containing Suwannee River Fulvic acid (SRFA), and wastewater. A higher sensitivity for most target carbonyl compounds was achieved compared to previous derivatisation methods. Moreover, the method allowed the identification of known and unknown carbonyl compounds. 8 out of 17 target carbonyl compounds were consistently detected above limits of quantification (LOQs) in most ozonated samples. Generally, the concentrations of the 8 detected target compounds decreased in the order: formaldehyde > acetaldehyde > glyoxylic acid > pyruvic acid > glutaraldehyde > 2,3-butanedione > glyoxal > 1-acetyl-1-cyclohexene. The DOC concentration-normalised formation of carbonyl compounds during ozonation was higher in wastewater and SRFA-containing water than in lake water. The specific ozone doses and the type of the dissolved organic matter (DOM) played a predominant role for the extent of formation of carbonyl compounds. Five formation trends were distinguished for different carbonyl compounds. Some compounds were produced continuously upon ozonation even at high ozone doses, while others reached a maximum concentration at a certain ozone dose above which they decreased. Concentrations of target and peak areas of non-target carbonyl compounds during full-scale ozonation at a wastewater treatment plant showed an increase as a function of the specific ozone dose (sum of 8 target compounds ∼ 280 µg/L at 1 mgO3/mgC), followed by a significant decrease after biological sand filtration (> 64–94% abatement for the different compounds). This highlights the biodegradability of target and non-target carbonyl compounds and the importance of biological post-treatment.

Use of Trifluoro-Acetate Derivatives for GC-MS and GC-MS/MS Quantification of Trace Amounts of Stera-3β,5α,6β-Triols (Tracers of Δ5-Sterol Autoxidation) in Environmental Samples.

Stera-3β,5α,6β-triols make useful tracers of the autoxidation of Δ5-sterols. These compounds are generally analyzed using gas chromatography-mass spectrometry (GC-MS) after silylation. Unfortunately, the 5α hydroxyl groups of these compounds, which are not derivatized by conventional silylation reagents, substantially alter the chromatographic properties of these derivatives, thus ruling out firm quantification of trace amounts. In this work, we developed a derivatization method (trifluoroacetylation) that enables derivatization of the three hydroxyl groups of 3β,5α,6β-steratriols. The derivatives thus formed present several advantages over silyl ethers: (i) better stability, (ii) shorter retention times, (iii) better chromatographic properties and (iv) mass spectra featuring specific ions or transitions that enable very low limits of detection in selected ion monitoring (SIM) and multiple reaction monitoring (MRM) modes. This method, validated with cholesta-3β,5α,6β-triol, was applied to several environmental samples (desert dusts, marine sediments and particulate matter) and was able to quantify trace amounts of 3β,5α,6β-steratriols corresponding to several sterols: not only classical monounsaturated sterols (e.g., cholesterol, campesterol and sitosterol) but also, and for the first time, di-unsaturated sterols (e.g., stigmasterol, dehydrocholesterol and brassicasterol).

Design, synthesis and antifungal activities of novel cis-enamides via intermediate derivatization method

On the basis of the structure of natural product lansiumamide B (1), a total of 27 novel cis-enamide compounds were designed and synthesized via Intermediate Derivatization Method. Their chemical structures were characterized by 1H and 13C nuclear magnetic resonance and high-resolution mass spectrometry. The in vitro antifungal activities against Sclerotinia sclerotiorum, Thanatephorus cucumeris and Botrytis cinerea were evaluated by the mycelium linear growth rate method. Most of the compounds showed some activity against each of the fungi at 25 or 50 μg/mL. The relationship between structure and antifungal activity was also discussed, which showed the cinnamic double bond was critical to maintain the antifungal activity. Notably, among the title compounds, 3e and 3h could inhibit mycelia growth of Botrytis cinerea by approximately 50% (EC50) at 39.17 and 41.25 μg/mL respectively, which showed better antifungal activity than lansiumamide B (1) with more concise chemical structure. The present study pointed out the correct direction for the development and optimization of lansiumamide B derivatives as potential inhibitors of pathogenic fungi.

Quantification of short-chain fatty acids in human stool samples by LC-MS/MS following derivatization with aniline analogues

The gut microbiome produces a range of short chain fatty acids (SCFA) crucially linked with diet and nutrition, metabolism, gastrointestinal health and homeostasis. SCFA are primarily measured using gas or liquid chromatography-mass spectrometry (LC/MS) after undergoing chemical derivatization. Here we assess the merits of a derivatization protocol using aniline and two aniline analogues (3-phenoxyaniline and 4-(benzyloxy)aniline) for the targeted LC-MS/MS quantification of nine SCFA (acetic, propionic, butyric, valeric, caproic acid, isobutyric, isovaleric, 2-methylbutyric, and 2-ethylbutyric acid). Evaluation of product ion spectra and optimization of MS detection conditions, provided superior detection sensitivity for 3-phenoxyaniline and 4-(benzyloxy)aniline compared to aniline. We developed a facile SCFA derivatization method using 3-phenoxyaniline under mild reaction conditions which allows for the simultaneous quantification of these SCFA in human stool samples in under eleven minutes using multiple reaction monitoring LC-MS/MS. The method was successfully validated and demonstrates intra- and inter-day accuracy (88.5–103% and 86.0–109%) and precision (CV of 0.55–7.00% and 0.33–9.55%) with recoveries (80.1–87.2% for LLOQ, 88.5–93.0% for ULOQ) and carry-over of (2.68–17.9%). Selectivity, stability and matrix effects were also assessed and satisfied validation criteria. Method applicability was demonstrated by analysing SCFA profiles in DNA-stabilized human stool samples from newly diagnosed colorectal cancer patients prior to surgery. The development of this improved method and its compatibility to measure SCFAs from DNA-stabilized stool will facilitate studies investigating the gut microbiome in health and disease.

Rapid Detection of Estrogens in Cosmetics by Chemical Derivatization and Paper-Spray Ionization Mass-Spectrometry.

Estrogens in personal care products are harmful to customers. Conventional methods such as HPLC and LC-MS require tedious sample pretreatment and long analytical time. Paper-spray ionization mass spectrometry (PSI-MS) is a powerful tool for the determination of compounds with little time and minimal pretreatment procedures. Since most estrogens show poor responses in PSI-MS, we developed a chemical derivatization and PSI-MS method to determinate three estrogens: estradiol, estriol and ethinyloestradiol with estradiol valerate as the internal standard (I.S.). After derivatization with 2-fluoro-1-methyl-pyridinium-p-toluene-sulfonate, the three estrogens could be quantified in seconds. This method showed good linearity in the range of 0.1~30 μg·mL-1, with R2 > 0.999. Their recovery results were all between 85%~115%. The limits of detection (LOD) were 0.04 μg·mL-1, 0.02 μg·mL-1 and 0.02 μg·mL-1 for estradiol, estriol and ethinyloestradiol respectively, which improved around 200, 2000, and 900 times compared to non-derivative PSI-MS. The method could quantitatively determine estrogens in cosmetics.

Evaluation of the dissolving ability of cellulosic pulps: investigation of a novel method using light scattering follow-up during classical cellulose carbanilation

Abstract The aim of the present study is to investigate the dissolving ability of a cellulosic substrate using a derivatization method, i.e. cellulose tricarbanilation and the follow-up by dynamic light scattering (DLS), for particle size measurement. The dissolving behavior of six commercial pulps, selected for their different nature and properties, were compared to the Fock test, and the analysis was completed by other methods for substrate characterization: crystallinity (XRD), DPv (in CuED), sugar analysis, molecular weight distribution (MWD) of cellulose by HPSEC-multidetectors (done on the cellulose tricarbanilates), and solubility in NaOH:urea:water. The proposed carbanilation/DLS method resulted practical and suitable for evaluating the dissolving ability of the different pulps – including hemicelluloses-containing kraft pulps – and allowed to discriminate the samples, contrary to the Fock test. Comparison and assessment of the relevance of the different methods are finally discussed.

Recent Advances in Biologic Therapeutic N-Glycan Preparation Techniques and Analytical Methods for Facilitating Biomanufacturing Automation

N-glycosylation is a post-translational modification that occurs during the production of monoclonal antibody (mAb) therapeutics. During production of mAb based therapeutics the use of various hosts and cell culture additives attribute to glycan heterogeneity. The safety and efficacy of monoclonal antibodies with mechanism of actions that utilize Fc effector functions can be negatively impacted by glycan heterogeneity and thus is often considered a critical quality attribute (CQA). In this mini review, we discuss recent advances in mAb sample preparation specifically focused on denaturation, enzymatic processing, and released glycans derivatization methods. Additionally, we review the recent advances in characterization of released and intact N-glycans using chromatography, capillary electrophoresis, and mass spectrometry techniques with a focus on rapid, automated approaches that support analysis of glycosylation profiles of biopharmaceuticals. We delve into advances within sample preparation techniques that allow for rapid and robust sample preparation as well as how these techniques are being used for innovative at-line high-throughput screening and process analytical technology (PAT). The future of biomanufacturing is focused on decreasing process costs while increasing process understanding and quality for novel biologic candidates and biosimilars. Therefore, advances in PAT for biotherapeutics will positively influence current manufacturing practices and enable further bioprocess automation.

Gas Chromatography Fingerprint of Martian Amino Acids before Analysis of Return Samples

Within the perspective of the current and future space missions, the detection and separation of building blocks such as amino acids are important subjects which are becoming fundamental in the search for the origin of life and traces of life in the solar system. In this work, we have developed and optimized a strategy adapted to space experimentation to detect the presence of amino acid-like compounds using gas chromatography coupled to mass spectrometry (GC-MS). Selected derivatization methods meet the instrument design constraints imposed on in situ extraterrestrial experiments. Coupled to a fast selective extraction, GC analysis would be highly efficient for the detection of organic materials. In the future, the corresponding GC-MS TIC could facilitate simple and fast selection of sediments/dust samples onboard GC-MS-equipped rovers for sample return-to-Earth missions.