This week on ChromatographyOnline.com, we highlight sustainable sample preparation alongside the transformative impact of AI and machine learning in chemical analysis, and explore advanced methodologies like ion mobility-HRMS and HPLC for tackling complex real-world challenges.
A study identified invasive Burmese pythons as effective biological sentinels for monitoring chemical pollution in the Florida Everglades. Researchers analyzed liver samples from 67 pythons using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) to track 30 per- and polyfluoroalkyl substances (PFAS).
German researchers used gas chromatography-mass spectrometry (GC–MS) and liquid chromatography-mass spectrometry (LC–MS) to analyze urinary and plasma steroid hormones in a female athlete, revealing cycle-dependent fluctuations in androgen levels during a natural menstrual cycle, with peaks around ovulation and declines in the luteal phase. In contrast, hormonal contraceptive use suppressed androgen variability, demonstrating the value of chromatographic techniques for sensitive monitoring of endocrine changes relevant to athletic performance and physiology.
To investigate how permanent chemical hair straightening influences the accuracy of hair drug testing using liquid chromatography–tandem mass spectrometry (LC-MS/MS), researchers analyzed hair samples before and after treatment with an alkaline straightener (ammonium thioglycolate), measuring levels of the endogenous compound gamma-hydroxybutyrate and the drug alprazolam. The study emphasizes the need for careful interpretation of LC-MS/MS hair analysis results and systematic documentation of cosmetic treatments in forensic and toxicological investigations, particularly when detecting low-level substances.
A mass balance and pharmacokinetic study of fezolinetant in healthy postmenopausal women employed high-performance liquid chromatography (HPLC) with radioactivity detection alongside liquid chromatography–tandem mass spectrometry (LC–MS/MS) to enable detailed metabolite profiling and structural elucidation. Overall, chromatographic techniques were central to quantifying drug disposition, identifying metabolic routes, and supporting the clinical development of this non-hormonal therapy for vasomotor symptoms.
To address the need for objective and non-invasive methods to measure workplace stress, a recent study evaluated metabolite profiling of mouth-rinsed water. Researchers using capillary electrophoresis-mass spectrometry (CE-MS) and liquid chromatography-mass spectrometry (LC-MS) analyzed 559 analytes from 32 participants categorized into high-stress and control groups.
Controlling the "heat" or pungency levels in chili peppers (Capsicum annuum) is a major challenge for breeders due to complex genetic inheritance. To address this, researchers are using high-performance liquid chromatography (HPLC) to precisely quantify capsaicin and dihydrocapsaicin levels. By combining these accurate chemical measurements with genomic prediction (GP) models, scientists can now better predict the spice levels of offspring based on parental data.
Gas chromatography-mass spectrometry (GC–MS), liquid chromatography-mass spectrometry (LC–MS), and inductively coupled plasma (ICP)-based techniques were applied to characterize extractables and potential leachables from polyurethane-insulated deep brain stimulation probes, comparing polyether urethane (PEU) and polycarbonate urethane (PCU) after prolonged exposure to a brain phantom.
Researchers used high-performance liquid chromatography–mass spectrometry (HPLC–MS) to perform targeted metabolomic analysis of urine samples from children with autism spectrum disorder (ASD) and healthy controls. By focusing on metabolites associated with the microbiota–gut–brain axis, researchers identified distinct biochemical patterns that differentiate ASD from typical development. The chromatography-based approach enabled precise and reliable measurement of seven key metabolites, highlighting its value over broader, non-targeted methods.
A recent paper introduced what the authors described as “an uncertainty-aware graph-based neural network that predicts retention times across multiple column chemistries and buffer pH conditions. LCGC International spoke to some of the authors of this paper, including corresponding author Pankaj Aggarwal, about their work.
Top articles published this week include a two part discussion on slalom chromatography, a look at the current analytical procedure lifecycle practices, and the utility of liquid chromatography coupled with mass spectrometric detection (LC–MS) for analysis of oligonucleotides (ONs).
Headspace solid-phase microextraction coupled with GC–MS (HS-SPME/GC-MS), integrated with machine learning, enabled comprehensive profiling of 127 volatile compounds across multiple vinegar types. Random Forest modeling achieved high classification accuracy, identifying key aroma markers and demonstrating the power of chromatographic–data science workflows for differentiating fermented food products.
A dual-injection, single-run liquid chromatography–high-resolution mass spectrometry (LC-HRMS) method enabled simultaneous profiling of phenolic and lipophenolic compounds in olive oil by-products. The approach achieved efficient separation and identification of over 40 compounds, overcoming solubility challenges and advancing high-throughput characterization of bioactive metabolites for sustainable valorization applications.
Gas chromatography–mass spectrometry (GC–MS) analysis of cotton headspace volatiles showed that plant growth-promoting rhizobacteria consortia alter emission profiles linked to reduced Spodoptera exigua oviposition. Key compounds, including terpenes and green leaf volatiles, mediated pest avoidance behavior, highlighting GC–MS as a tool for advancing integrated pest management strategies.
Headspace gas chromatography–mass spectrometry (GC-MS) analysis of paired maternal and umbilical cord blood demonstrated that induction-to-delivery time strongly influences fetal sevoflurane exposure. While maternal anesthetic levels did not predict fetal concentrations, longer delivery intervals increased transfer, highlighting timing as a critical factor in managing anesthetic exposure during cesarean delivery.
Researchers utilized high-resolution liquid chromatography coupled with tandem mass spectrometry (LC-HRMS/MS) and chemometric modeling to profile the leaf metabolomes of three taxonomically complex Brazilian Vanilla species. By identifying 17 core discriminating biomarkers, this untargeted metabolomic approach successfully established species-specific metabolic fingerprints, providing a robust new strategy for chemotaxonomic classification and species authentication.
Researchers using gas chromatography–mass spectrometry (GC-MS) to study the gases released from heat-treated spruce wood found that heating the wood—especially at higher temperatures—greatly reduces the amount of these gases, which can affect indoor air quality.
As more people choose plant-based milks like oat, almond, soy, and coconut, new challenges arise in ensuring these drinks are safe—especially in preventing accidental allergen exposure. While factory checks are standard, they don't address risks at the point of consumption. A recent study proposed a "digital nose" using AI to "smell" and verify milk quality in real-time. To calibrate these sensors, researchers used gas chromatography-mass spectrometry coupled with solid-phase microextraction (GC-MS-SPME) as the gold-standard reference to accurately identify the unique scent profiles of each milk type.
To address the growing challenge of trace contaminants surviving standard water treatment, Portuguese researchers have developed and validated a highly sensitive solid-phase extraction ultra-high performance liquid chromatography coupled to tandem mass-spectrometry (SPE-UHPLC-MS/MS) method to monitor 23 microscopic pollutants—including pharmaceuticals, pesticides, and UV-filters—in drinking water. The method successfully identified four target compounds at safe residual levels, providing vital data to support emerging European Union water safety directives and filling a critical gap in regional water monitoring.
Researchers combined gas chromatography-ion mobility spectrometry (GC-IMS), headspace solid-phase microextraction (HS-SPME), stir bar sorptive extraction (SBSE), and gas chromatography-olfactometry-mass spectrometry (GC-O-MS) to characterize volatile compounds in cigar tobacco leaves from different regions. Fifteen key aroma-active compounds were identified, defining sensory profiles such as fruity, citrus, and chocolate notes, supporting improved raw material selection and future predictive models for cigar aroma development.
A recent study shows that integrating multipass cyclic ion mobility spectrometry into liquid chromatography-high-resolution mass spectrometry improves detection and separation of toxic plant-derived pyrrolizidine alkaloids, including previously indistinguishable epimers, in complex food samples. LCGC International spoke to Laura Carbonell-Rozas, lead author of that paper, about the study.
Researchers utilized untargeted liquid chromatography-tandem mass spectrometry (LC-MS/MS) and metagenomic sequencing to analyze the gut microbiota and fecal metabolites of captive Asian elephants. Seeking to understand reproductive challenges in this endangered species, the team compared pregnant females, non-pregnant adults, and subadults. Ultimately, these multi-omics insights aim to guide better dietary and health management to support the conservation and breeding of captive Asian elephants.
This week highlights advances in food authenticity research, AI applications in analytical chemistry, REIMS for pork classification, improved GC×GC sensitivity, and greener SFC workflows.
A pilot study conducted by researchers from Texas State University and Yale utilized liquid chromatography-tandem mass spectrometry (LC-MS/MS) to analyze whole blood samples from active-duty firefighters for 24 distinct per- and polyfluoroalkyl substances (PFAS). The analysis successfully quantified key analytes, revealing a direct negative association between PFOS concentrations and cognitive processing speed. This research highlights the essential role of advanced LC-MS/MS techniques in uncovering the hidden occupational hazards and neurotoxicological impacts of "forever chemicals" on first responders.
Reverse-phase high-performance liquid chromatography (HPLC) equipped with fluorescence detection was used to measure peripheral concentrations of tryptophan (Trp), serotonin (5-HT), and 5-hydroxyindoleacetic acid (5-HIAA) in patients with relapsing-remitting multiple sclerosis (RRMS).
Gas chromatography-mass spectrometry (GC-MS) was used to analyze volatile compounds across various commercial smoked products, tracking the specific chemical drivers of smoky flavors.
Researchers used liquid chromatography-tandem mass spectrometry (LC-MS/MS) to measure over 200 environmental exposures in the blood of adults from an industrialized region in northern China. The study found that elevated levels of specific endocrine-disrupting chemicals and persistent organic pollutants were significantly associated with an increased likelihood of being overweight, emphasizing the potential impact of complex chemical mixtures on obesity.
Researchers employed ultra-high-performance liquid chromatography (UHPLC) with orbital trap mass spectrometry and liquid chromatography-tandem mass spectrometry (LC-MS/MS) to conduct a multi-omics analysis of patients with coronary heart disease (CHD). The study identified significant gut microbiota dysbiosis, alongside 32 differentially expressed metabolites and 38 differentially expressed proteins. These findings reveal distinct metabolic pathway alterations that could serve as potential diagnostic biomarkers and novel therapeutic targets for early CHD detection and intervention.
Liquid chromatography-mass spectrometry (LC-MS) was used to perform comprehensive, nontargeted metabolomic profiling on serum samples from adult patients with type 1 diabetes (T1D). The data establishes LC-MS as a powerful diagnostic tool to help prevent the common misdiagnosis of adult T1D as type 2 diabetes.
Following 2025 FDA initiatives to ensure the safety of children's foods, researchers developed a highly sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to detect eight prohibited acidic and basic synthetic dyes in candies and cereals. Although no unauthorized dyes were found in the analyzed samples, the study demonstrates that robust, routine analytical screening is essential to verify labeling accuracy, maintain regulatory compliance, and protect vulnerable populations.
