Chromatographia最新文献

{"title":"Flameless Operating Mode for Improved Multiple Flame Photometric Detection in Gas Chromatography","authors":"Bao Nguyen,&nbsp;Kevin B. Thurbide","doi":"10.1007/s10337-024-04335-x","DOIUrl":"10.1007/s10337-024-04335-x","url":null,"abstract":"<div><p>A novel flameless operating mode is introduced, which improves the response of a multiple flame photometric detector (mFPD). The mFPD normally has analyte travel through 4 ‘worker’ flames in series before entering a final ‘analytical’ flame where its emission is monitored. Here, it is found that when the analytical flame is not ignited, background luminescence is reduced over 30 times and the strong analyte chemiluminescence of the worker flames can be made to extend a large distance (~ 10 flame widths) into the analytical flame region where it is detected. This occurs for phosphorous (HPO*), quadratic sulfur (S₂*), and linear sulfur (HSO*) emission. Conversely, carbon emission resides inside the worker flames and yields a small negative signal. As a result, very good selectivity over carbon is observed, and improved minimum detectable limits (MDL) of 4 pg S/s (S₂*) and 0.3 pg P/s (HPO*) are obtained, which are up to 20 times lower than previous values reported for the mFPD. Further, linear sulfur (HSO*) yields an MDL of 6 pg S/s, which is over 3 times lower than values reported for other FPDs. Due to the worker flames present in this mode, other benefits of regular mFPD operation are maintained, like uniform analyte response and large quenching resistance. In application, a trace benzothiophene analyte is readily detected within a concentrated diesel fuel matrix in the flameless mFPD mode, while no response is observed in the conventional FPD mode. Results indicate that this flameless operating mode is advantageous for sulfur and phosphorous analysis.</p><h3>Graphical Abstract</h3><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"87 6","pages":"363 - 373"},"PeriodicalIF":1.2,"publicationDate":"2024-04-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140658460","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Simultaneous Determination and Drug–Drug Interaction Study of Losartan and Aprepitant Through Pharmacokinetic Approach in Rat Plasma by UHPLC–QqQ-MS/MS","authors":"Shraddha Naresh Katarpawar,&nbsp;Kandula Jony Susanna,&nbsp;V. V. S. Prasanna Kumari Rayala,&nbsp;P. Radhakrishnanand","doi":"10.1007/s10337-024-04332-0","DOIUrl":"10.1007/s10337-024-04332-0","url":null,"abstract":"<div><p>Losartan is an anti-hypertensive drug that belongs to the class of angiotensin-II receptor blockers that act by inhibiting the binding of angiotensin II to its receptor. Aprepitant belongs to the class of neurokinin receptor-1 receptor blockers used to treat nausea and vomiting. In the case of severe hypertension, there are the majority of predominant symptoms occurring but one such symptom is nausea and vomiting. This condition may potentially be treated by a combination of losartan and aprepitant, but there is no information about the pharmacokinetic interactions for this combination. When losartan and aprepitant are taken concomitantly there may be a chance that these two drugs may alter the pharmacokinetics of each other. Thus, the effects of both the drugs were assessed on each other. To assess the preclinical pharmacokinetic drug–drug interaction a rapid, simple, and sensitive approach for the simultaneous estimation of losartan and aprepitant in rat plasma by LC–QqQ-MS/MS has been developed and validated. The separation was done on Agilent ZORBAX Eclipse Plus C18 (4.6 mm × 100 mm, 3.5 µm) by gradient elution using 0.1% (<i>v/v</i>) formic acid in water and acetonitrile. Multiple reaction monitoring was performed using a positive ionization mode. The precursor and product ions for losartan, aprepitant, and telmisartan (internal standard) were <i>m/z</i> 423.2 → 207.0, <i>m/z</i> 535.2 → 277.0, and, <i>m/z</i> 515.3 → 276.1, respectively. The proposed method was validated in accordance with USFDA bioanalytical guidelines. The method was found linear, accurate and sensitive to estimate the losartan and aprepitant in rat plasma with the lowest limit of quantification of 1 ng/mL. The pharmacokinetic parameters like half-life, <i>T</i>_max and the area under the curve for aprepitant have been significantly affected when administered with losartan and vice versa. These results provide insights for futuristic investigation at the pharmacodynamic level of drug–drug interactions for this combination.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"87 6","pages":"419 - 432"},"PeriodicalIF":1.2,"publicationDate":"2024-04-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140675445","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Comparison of Testosterone Extraction from Human Plasma Using MOFs (MIL-53(Al) and ZIF-8)-Based D-µ-SPE Coupled to HPLC–UV","authors":"Somaye Akbari,&nbsp;Azra Takhvar,&nbsp;Effat Souri,&nbsp;Reza Ahmadkhaniha,&nbsp;Ali Morsali,&nbsp;Mohammad Reza Khoshayand,&nbsp;Mohsen Amini,&nbsp;Alireza Taheri","doi":"10.1007/s10337-024-04329-9","DOIUrl":"10.1007/s10337-024-04329-9","url":null,"abstract":"<div><p>A novel technique utilizing metal–organic frameworks (MOFs), namely MIL-53(Al) and ZIF-8, has been developed for the extraction of testosterone from human plasma through dispersive micro-solid phase extraction (D-µ-SPE or DMSPE). The synthesized MOFs were subjected to characterization via Fourier transform infrared spectroscopy (FT-IR), powder X-ray diffraction (PXRD), and scanning electron microscopy (SEM). The parameters affecting the extraction were optimized by response surface methodology (RSM). The optimal extraction conditions were determined to be 15 min for contact time, 1 mg for MIL-53(Al) amount, and 0.23% (w/v) for NaCl concentration. For ZIF-8, a contact time of 22 min, a sorbent amount of 5.4 mg, and a salt concentration of 0.34% (w/v) were obtained. Batch absorption studies were conducted to find appropriate kinetic and isotherm models. The results indicated that while testosterone absorption was favorable in both cases, MIL-53 (Al) had a higher absorption capacity than ZIF-8. Finally, the proposed method was subjected to analytical validation for determination of testosterone in plasma samples. Good analytical performance was achieved, including a dynamic range of 0.05–1 µg/mL using each of the sorbents. The precision (expressed as the relative standard deviation (RSD)) and accuracy (expressed as the percentage error) of the method for testosterone and MIL-53(Al) were found to be 3.40% and 2.79%, respectively, while for testosterone and ZIF-8, they were 4.24% and 4.22%, respectively. The method effectively extracted 97% and 96% of testosterone from spiked plasma samples using MIL-53(Al) and ZIF-8, respectively.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"87 6","pages":"385 - 398"},"PeriodicalIF":1.2,"publicationDate":"2024-04-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140676821","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"HPLC Method for Simultaneous Identification and Quantification of Enrofloxacin, Bromhexine*HCl and Their Related Substances/Degradation Products, in Veterinary Pharmaceutical Product, Bromflovet","authors":"Maria Neagu,&nbsp;Vasile Cornel Rusu,&nbsp;Iosif Cadleti,&nbsp;Ionel-Bogdan Cioroiu,&nbsp;Marius Niculaua,&nbsp;Constantin-Bogdan Nechita,&nbsp;Aurel-Marian Chirita,&nbsp;Valeriu V. Cotea","doi":"10.1007/s10337-023-04310-y","DOIUrl":"10.1007/s10337-023-04310-y","url":null,"abstract":"<div><p>This study aims to develop a chromatographic analytical method, for separation, identification and quantification of degradation products, in veterinary finished product with two active substances enrofloxacin and bromhexine hydrochloride. Analytical method used an Agilent Eclipse Plus C18 column (150 × 4.6 mm, 5 µm particle size) and a mobile phase A consisted of 2.5% (v/v) phosphoric acid adjusted to pH 2.3 with triethylamine and mobile phase B was acetonitrile. Elution was in a gradient mode with total chromatographic time being 21 min. Detection was performed at 248 nm for bromhexine hydrochloride and at 272 nm for enrofloxacin. The method was developed to assure the separation of impurities of enrofloxacin and bromhexine hydrochloride. Specificity in relation with degradation products revealed up to 20 impurities for enrofloxacin and 7 impurities related with bromhexine hydrochloride. The spectra of impurities were chosen among the compounds found in forced degradation studies. Method validation was performed according to VICH GL 2—validation of analytical procedures and included selectivity/specificity, linearity, accuracy, precision, limit of quantification, limit of detection, robustness, and system suitability. Linearity was between 0.015 and 0.06 mg/mL for enrofloxacin and 0.001125–0.005625 mg/mL for bromhexine hydrochloride. Limit of quantification was 0.00292 mg/mL for enrofloxacin and 0.001103 mg/mL for bromhexine hydrochloride. These limits assured method performance, because they are under the reporting threshold of 0.3% as stated in VICH GL11 Impurities in new veterinary medicinal products which is 0.30%. Recovery was calculated on three concentrations for every compound and was 102.99% for enrofloxacin and 102.91% for bromhexine hydrochloride. In terms of intermediate precision, a relative maximum deviation of 2.50% was obtained for area and retention time using two analysts in two different days of application.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"87 5","pages":"309 - 323"},"PeriodicalIF":1.2,"publicationDate":"2024-04-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140625551","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Application High-Performance Thin-Layer Chromatography with Controlled Eluent Velocity to Determine Fingerprints of Various Poplar Species Buds Extracts: Optimization of Operating Variables","authors":"Aneta Hałka-Grysińska,&nbsp;Beata Polak,&nbsp;Dominika Warianek,&nbsp;Loretta Pobłocka-Olech,&nbsp;Mirosława Krauze-Baranowska,&nbsp;Tadeusz H. Dzido","doi":"10.1007/s10337-024-04333-z","DOIUrl":"10.1007/s10337-024-04333-z","url":null,"abstract":"<div><p>The study used the prototype device enabling the development of isocratic and gradient thin-layer chromatograms with controlled eluent velocity to obtain fingerprints of extracts from buds of various poplar species. This equipment can deliver an eluent to virtually any place on the adsorbent layer of the chromatographic plate. Moreover, the composition of a mobile phase can be easily modified even when the chromatogram is developing. This paper shows the effect of various operating variables of the prototype in a normal phase system, e.g., eluent velocity and composition, on the chromatographic behavior of the mixture. The prototype’s results were compared to conventional TLC development in horizontal DS chambers. The UV light (366 nm) was used to detect the solute zones and document both systems. The results prove that the prototype device has great potential in plant material standardization. The mobile phase gradient improves the separation of the bands of strongly retained solutes. Additionally, this fact does not enhance the blurring of low-retained bands.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"87 6","pages":"399 - 406"},"PeriodicalIF":1.2,"publicationDate":"2024-04-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10337-024-04333-z.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140629705","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Characterization and Application of Membrane-emulsified HLB Microspheres for Quantification of 25-Hydroxy Vitamin D2 and 25-Hydroxy Vitamin D3 in Serum by UPLC-MS/MS","authors":"Jihua Zhang,&nbsp;Zishan Gong,&nbsp;Hang Tie,&nbsp;Yanchun Wang,&nbsp;Xuan Wang,&nbsp;Weixiang Zhai,&nbsp;Qiaoyun Guo,&nbsp;Wenhui Wu,&nbsp;Jiyang Liu,&nbsp;Liang Xu,&nbsp;Wenli Jing,&nbsp;Shuo Zhang","doi":"10.1007/s10337-024-04331-1","DOIUrl":"10.1007/s10337-024-04331-1","url":null,"abstract":"<div><p>Membrane emulsification can obtain microspheres with relatively uniform particle size and pore size, which has unique advantages in the synthesis of polymer microsphere adsorbents and the enrichment and separation of organic compounds. In this study, the Hydrophilic Lipophilic Balance (HLB) solid phase extraction microspheres were prepared by membrane emulsification technique and was used in the pretreatment of samples to detect 25-hydroxy vitamin D₂ (25OH-VD₂) and 25-hydroxy vitamin D₃ (25OH-VD₃) in serum by UPLC-MS/MS for the first time. To confirm the efficacy of membrane-emulsified (ME) HLB microspheres, three types of microspheres, including ME HLB microspheres, non-membrane-emulsified (non-ME) HLB microspheres and commercial HLB microspheres, were compared for the pretreatment of 25OH-VD₂ and 25OH-VD₃. The performance of HLB microspheres was characterized based on the sample recovery values acquired by UPLC-MS/MS analysis. Results showed that among the three types of microspheres, ME HLB microspheres showed the best performance and demonstrated good adsorption properties for 25OH-VD₂ and 25OH-VD₃. The recoveries range of 25OH-VD₂ and 25OH-VD₃ were 96.7–101.4 and 98.7–104.9%, respectively, and the coefficients of variation were 0.67–1.24 and 1.39–2.28%, respectively, which were superior to those of commercial HLB microspheres and non-ME HLB microspheres. Additionally, due to their excellent homogeneity, the ME HLB microspheres exhibited good precision in the determination of low values of 25OH-VD₂ and 25OH-VD₃, indicating accurate and simple detection of 25OH-VD₂ and 25OH-VD₃ with a broad potential for further development.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"87 5","pages":"351 - 361"},"PeriodicalIF":1.2,"publicationDate":"2024-04-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140588249","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Measurement of Distribution Constants Between Air and Solid Substrates Using Gas Chromatography for Quantification of Hydrocarbons in Solid Substrates via Headspace-Solid Phase Microextraction","authors":"Joonyeong Kim,&nbsp;Jihnhee Yu","doi":"10.1007/s10337-024-04328-w","DOIUrl":"10.1007/s10337-024-04328-w","url":null,"abstract":"<div><p>This study focused on the chromatographic measurements of the distribution constants of hydrocarbons at the air–solid interface for indirect quantification of the hydrocarbon compositions in solid substrates via headspace-solid phase microextraction (HS-SPME). Packed column gas chromatography and other experimental data were used to measure the distribution constants of six hydrocarbons (<i>n</i>-heptane, <i>n</i>-octane, <i>n</i>-nonane, toluene, <i>p</i>-xylene, and <i>1,2,4</i>-trimethylbenzene) between the headspace (HS) and two solid substrates (cardboard and cotton fabric) at 60 and 90 °C. To validate the accuracies of the measured distribution constants in this work, model HS samples were prepared in vials containing known amounts of solid substrates and a mixture of vaporized hydrocarbons at 60 and 90 °C. These HS samples were analyzed with gas chromatography using both direct vapor analysis and HS-SPME. The experimental hydrocarbon compositions of HS samples were compared with the calculated HS compositions from the measured distribution constants and other experimental parameters. The Wilcoxon signed-rank test results indicated that the calculated hydrocarbon compositions of the model samples were comparable with the experimental hydrocarbon compositions. This work suggests that gas chromatographic measurements using packed columns can provide a reliable and convenient method for measuring the distribution constants of hydrocarbons between air and various solid substrates.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"87 5","pages":"285 - 294"},"PeriodicalIF":1.2,"publicationDate":"2024-04-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140588267","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Development of a Green Water-Induced Restricted Access Supramolecular Solvent Microextraction Method for Highly Improved Determination of Pesticides with a Wide Range of Polarity in Water Samples and Cereal Flours","authors":"César Ricardo Teixeira Tarley,&nbsp;Luciane Effting,&nbsp;Ismael Rodrigues Amador,&nbsp;Maikon Thiago do Nascimento","doi":"10.1007/s10337-024-04330-2","DOIUrl":"10.1007/s10337-024-04330-2","url":null,"abstract":"<div><p>A novel green microextraction supramolecular (SUPRA)-based method for simultaneous preconcentration of seven pesticides, acetamiprid, azoxystrobin, bifenthrin, carbendazim, chlorpyrifos, imidacloprid, and tebuconazole, in water samples and cereal flours with further determination by HPLC-DAD was developed. The method uses 113 µL of 1-decanol as amphiphilic extractor and 500 µL of tetrahydrofuran as disperser solvent. To perform the method optimization, a 2⁵ factorial design and Doehlert design combined with Derringer–Suich desirability function and response surface methodology were used. The microextraction of the pesticides was carried out at pH 6.3 in the presence of 5% NaCl (w/v), low vortex-assisted extraction time (30 s) and it was provided high preconcentration factors (3.6–266.1), and low LOQs (8.98–29.92 µg L⁻¹). The intra-day (<i>n</i> = 10) and inter-day (<i>n</i>  = 10) precision assessed as the percentage of relative standard deviation (%RSD) for concentrations of 50.0 and 200.0 µg L⁻¹ varied from 1.7 to 4.1%. The method was successfully applied to determine pesticides in river and lake water samples using external calibration curves. Considering the property of restricted access materials of SUPRAs, the microextraction method was also applied to the direct treatment of solid samples of wheat, oat, and rice flours. High recovery values in the range of 80–112% were obtained, thereby proving the absence of possible interference from matrix components.</p><h3>Graphical Abstract</h3><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"87 5","pages":"295 - 308"},"PeriodicalIF":1.2,"publicationDate":"2024-04-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140588189","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"HPLC–UV Monitored Photostability-Test of LE404 and Identification of the Degradation Products via NMR and LC–HRMS","authors":"Stephanie Zergiebel,&nbsp;Nico Ueberschaar,&nbsp;Jonathan Plentz,&nbsp;Andreas Seeling","doi":"10.1007/s10337-024-04323-1","DOIUrl":"10.1007/s10337-024-04323-1","url":null,"abstract":"<div><p>Dibenzoazecines are a new class of potential neuroleptics with a high potential for the treatment of schizophrenia. Initial stress tests indicated that the lead compound, LE404, decomposes when exposed to oxygen and sunlight. In this follow-up study, the influence of oxidative stress and photosensitivity was investigated in accordance with the ICH guidelines. These studies are of great importance for new APIs, as phototoxic and photoallergic reactions pose a significant risk to patients, especially with long-term medication, as it is not possible to completely avoid exposure to sunlight. Furthermore, the identification and prediction of the chemical lability of LE404 can be used to determine suitable storage conditions to prevent compound degradation. The effects of exposure of LE404 to a light source similar in spectrum and intensity to natural sunlight were investigated according to ICH-Q1B. Furthermore, the influence of oxidizing agents was investigated under exclusion of light. Two degradation products were identified. The extent and rate of degradation were continuously monitored using RP-HPLC–UV. Chromatographic separations were performed with a phenomenex™ Gemini 5 µm C18 (250 × 4.60 mm) column and acetonitrile/KH₂PO₄ buffer (4 mmol L⁻¹, pH 2.5) as mobile phase at 220 nm. The photodegradation product was isolated using semi-preparative RP-HPLC. The oxidation product was obtained by quantitative conversion of LE404 in hydrogen peroxide and subsequent purification by preparative TLC. The structures of both degradation products were elucidated using HR-MS/MS, 1D- and 2D-NMR as well as FT-IR spectroscopy. The characterization of the degradation products serves as the basis for subsequent investigations into their toxicity.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"87 5","pages":"339 - 349"},"PeriodicalIF":1.2,"publicationDate":"2024-04-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140588266","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Simultaneous Analysis of Formaldehyde and Methanol Emissions During Curing Reactions of Polyester-melamine Coatings","authors":"Elias Rippatha,&nbsp;Clemens Schwarzinger","doi":"10.1007/s10337-024-04325-z","DOIUrl":"10.1007/s10337-024-04325-z","url":null,"abstract":"<div><p>This paper introduces a new derivatization agent for the simultaneous quantification of formaldehyde and methanol during curing reactions of complex organic coatings. Formaldehyde emitted from a polyester-melamine coating is derivatized in a gas phase reaction with unsymmetrical dimethylhydrazine (UDMH) to form formaldehyde dimethylhydrazone (FDMH). UDMH and FDMH tend to degrade at temperatures above 200 °C rather fast. The applicability of derivatization agent and analyte as well as their degradation products are therefore discussed thoroughly. In this method curing temperatures of 150 °C with incubation times between 0.1 and 60 min are used to trigger crosslinking reactions. The emissions of formaldehyde and methanol are continuously quantified with headspace gas chromatography to obtain an emission trend. While one of the main sources of formaldehyde is the demethylolation during crosslinking, methanol is produced via hexamethoxymethylmelamine (HMMM) deetherification and as a condensation byproduct. The emission monitoring shows a high potential for comparative and mechanistic investigations. Results show good repeatability with low standard deviations (&lt; 7%) with a quantification limit of 2.09 µg for formaldehyde and 2.08 µg for methanol.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"87 5","pages":"275 - 283"},"PeriodicalIF":1.2,"publicationDate":"2024-04-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10337-024-04325-z.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140588186","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}