Linaclotide is an important peptide drug used to treat irritable bowel syndrome with constipation (IBS-C). However, structurally related impurities in peptide drugs can be generated during synthesis, storage, or transport, which compromise the quality and safety. Therefore, developing a highly sensitive analytical method for impurity detection is of great significance.
Methods
A liquid chromatography–high resolution mass spectrometry (LC-HRMS) method was developed. Linaclotide samples were directly analyzed using an Orbitrap mass spectrometer with an electrospray ionization (ESI) source operated in positive ion mode. Tandem mass spectrometry with collision-induced dissociation was utilized. The method leveraged high mass accuracy to identify and quantify structurally related peptide impurities in linaclotide samples from different manufacturers.
Results
The method was applied to characterize the peptide impurities in linaclotide study materials. In manufacturer A's material, [Des-Tyr14]-linaclotide was found at 0.453 mg/g. The same impurity was found in manufacturer B's material at 0.768 mg/g, as well as another impurity [endo-Ala9]-linaclotide at 0.555 mg/g.
Conclusions
The developed LC-HRMS method successfully addresses the challenge of determining structurally related peptide impurities in linaclotide. Its ability to characterize specific impurities provides a valuable complement to existing quality control strategies for peptide therapeutics.
{"title":"Identification and Quantification of Structurally Related Peptide Impurity in Linaclotide by Liquid Chromatography–High Resolution Mass Spectrometry","authors":"Jinlan Cheng, Tianji Zhang, Xinling Cui, Peize Wu, Ming Li, Wenrui Hu, Xueting Dai, Xuesong Feng","doi":"10.1002/rcm.70030","DOIUrl":"https://doi.org/10.1002/rcm.70030","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>Linaclotide is an important peptide drug used to treat irritable bowel syndrome with constipation (IBS-C). However, structurally related impurities in peptide drugs can be generated during synthesis, storage, or transport, which compromise the quality and safety. Therefore, developing a highly sensitive analytical method for impurity detection is of great significance.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>A liquid chromatography–high resolution mass spectrometry (LC-HRMS) method was developed. Linaclotide samples were directly analyzed using an Orbitrap mass spectrometer with an electrospray ionization (ESI) source operated in positive ion mode. Tandem mass spectrometry with collision-induced dissociation was utilized. The method leveraged high mass accuracy to identify and quantify structurally related peptide impurities in linaclotide samples from different manufacturers.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>The method was applied to characterize the peptide impurities in linaclotide study materials. In manufacturer A's material, [Des-Tyr<sup>14</sup>]-linaclotide was found at 0.453 mg/g. The same impurity was found in manufacturer B's material at 0.768 mg/g, as well as another impurity [endo-Ala<sup>9</sup>]-linaclotide at 0.555 mg/g.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>The developed LC-HRMS method successfully addresses the challenge of determining structurally related peptide impurities in linaclotide. Its ability to characterize specific impurities provides a valuable complement to existing quality control strategies for peptide therapeutics.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"40 7","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145987104","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Strahil Berkov, Rumen Denev, David Kok, Jean Paulo de Andrade, Boriana Sidjimova, Luciana R. Tallini, Laura Torras-Claveria, Ahmed Hussein, Jaume Bastida
Rationale
The search for novel natural compounds and the identification of known ones is a challenge for the scientists working in different fields of plant science. Due to its accessibility, GC–MS is the most frequently applied method for analysis of extracts and fractions from plants of the subfamily Amaryllidoideae (Amaryllidaceae s.s.), known as a source of molecules with potent anti-acetylcholinesterase, anti-tumour, and antiprotozoal activities.
Methods
Thirty-four standard alkaloids with haemanthamine- and crinine-type scaffolds were subjected to electron impact gas chromatography–mass spectrometry (GC–MS) to determine their fragmentation patterns. Additionally, underivatised and silylated alkaloid fractions from several Amaryllidoideae plants were also analysed by GC–MS.
Results
Most of the compounds showed excellent separation and specific MS fragmentation allowing rapid structural determination. The degree of saturation of ring C and the substituents at C3, C6, and C11 impact the fragmentation of these molecules. GC–MS allowed differentiation of the epimers at C3. Silylation of compounds with hydroxyl groups at C6 and C11 improved the resolution, especially of C6-OH epimers. Analyses of alkaloid fractions from different Amaryllidaceae plants resulted in the tentative identification of five new alkaloids on the basis of their fragmentation pattern and comparison of their mass spectra with those of standard compounds.
Conclusions
GC–MS can be effectively employed for the discovery of novel bioactive compounds and the identification of known ones, as well as for chemotaxonomic and chemoecological studies, among other applications, within the Amaryllidoideae subfamily.
{"title":"GC–MS of Some Haemanthamine- and Crinine-Type Amaryllidaceae Alkaloids","authors":"Strahil Berkov, Rumen Denev, David Kok, Jean Paulo de Andrade, Boriana Sidjimova, Luciana R. Tallini, Laura Torras-Claveria, Ahmed Hussein, Jaume Bastida","doi":"10.1002/rcm.70019","DOIUrl":"https://doi.org/10.1002/rcm.70019","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>The search for novel natural compounds and the identification of known ones is a challenge for the scientists working in different fields of plant science. Due to its accessibility, GC–MS is the most frequently applied method for analysis of extracts and fractions from plants of the subfamily Amaryllidoideae (Amaryllidaceae <i>s.s</i>.), known as a source of molecules with potent anti-acetylcholinesterase, anti-tumour, and antiprotozoal activities.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>Thirty-four standard alkaloids with haemanthamine- and crinine-type scaffolds were subjected to electron impact gas chromatography–mass spectrometry (GC–MS) to determine their fragmentation patterns. Additionally, underivatised and silylated alkaloid fractions from several Amaryllidoideae plants were also analysed by GC–MS.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>Most of the compounds showed excellent separation and specific MS fragmentation allowing rapid structural determination. The degree of saturation of ring C and the substituents at C3, C6, and C11 impact the fragmentation of these molecules. GC–MS allowed differentiation of the epimers at C3. Silylation of compounds with hydroxyl groups at C6 and C11 improved the resolution, especially of C6-OH epimers. Analyses of alkaloid fractions from different Amaryllidaceae plants resulted in the tentative identification of five new alkaloids on the basis of their fragmentation pattern and comparison of their mass spectra with those of standard compounds.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>GC–MS can be effectively employed for the discovery of novel bioactive compounds and the identification of known ones, as well as for chemotaxonomic and chemoecological studies, among other applications, within the Amaryllidoideae subfamily.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"40 7","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145983837","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Jordan A. G. Wostbrock, Drake Yarian, Isabella Chiaravalloti, Spencer R. Moller, Ruth E. Blake
Rationale
Increasingly, more laboratories are measuring the triple oxygen isotope values of phosphate. Standardization is key to having good interlaboratory results. Here, we present the triple oxygen isotope values of a suite of standards using fluorination and compare them with previously reported triple oxygen isotope values.
Methods
Silver phosphate (~2–3 mg) was fluorinated in nickel reaction vessels, and the resulting O2 was analyzed on a Thermo MAT 253 for the paired δ17O-δ18O value (Δ′17O). Although the δ18O and δ17O values were variable, the fluorination reaction progresses along a slope of ~0.528, indicating that the Δ′17O is constant when calculated using a λref = 0.528. The 18O/16O ratio was obtained using a TC/EA, and the δ17O value was corrected based on the measured Δ′17O value from fluorination and the δ18O values obtained on the TC/EA.
Results
We provide δ17O, δ18O, and Δ′17O values for the following silver phosphate standards: NBS120c, USGS80, USGS81, AGLox, and B2207. Two new standards are also reported and available for distribution. To report our values on the VSMOW2-SLAP2 scale, we measured common silicate standards: San Carlos Olivine, NBS28, NMQ, and SKFS that have been calibrated to VSMOW2-SLAP2. Our reported Δ′17O error for silver phosphate is 10 per meg, calculated using the average long-term standard deviation of our two most replicated standards.
Conclusions
We report the δ17O, δ18O, and Δ′17O values for a large suite of silver phosphate standards and present two new standards that can be used for interlaboratory calibration. Our results are reported on the VSMOW2-SLAP2 scale by measuring silicates on the same instrument with the same reference gas. The fluorination method in nickel reaction vessels is easily adapted to other laboratories that have fluorination lines. Only 2–3 mg of silver phosphate is needed for Δ′17O measurements when paired with δ18O values using the TC-EA technique.
{"title":"Fluorination of Silver Phosphate in Nickel Reaction Vessels for Triple Oxygen Isotope Analysis","authors":"Jordan A. G. Wostbrock, Drake Yarian, Isabella Chiaravalloti, Spencer R. Moller, Ruth E. Blake","doi":"10.1002/rcm.70016","DOIUrl":"https://doi.org/10.1002/rcm.70016","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>Increasingly, more laboratories are measuring the triple oxygen isotope values of phosphate. Standardization is key to having good interlaboratory results. Here, we present the triple oxygen isotope values of a suite of standards using fluorination and compare them with previously reported triple oxygen isotope values.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>Silver phosphate (~2–3 mg) was fluorinated in nickel reaction vessels, and the resulting O<sub>2</sub> was analyzed on a Thermo MAT 253 for the paired δ<sup>17</sup>O-δ<sup>18</sup>O value (Δ′<sup>17</sup>O). Although the δ<sup>18</sup>O and δ<sup>17</sup>O values were variable, the fluorination reaction progresses along a slope of ~0.528, indicating that the Δ′<sup>17</sup>O is constant when calculated using a λ<sub>ref</sub> = 0.528. The <sup>18</sup>O/<sup>16</sup>O ratio was obtained using a TC/EA, and the δ<sup>17</sup>O value was corrected based on the measured Δ′<sup>17</sup>O value from fluorination and the δ<sup>18</sup>O values obtained on the TC/EA.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>We provide δ<sup>17</sup>O, δ<sup>18</sup>O, and Δ′<sup>17</sup>O values for the following silver phosphate standards: NBS120c, USGS80, USGS81, AGLox, and B2207. Two new standards are also reported and available for distribution. To report our values on the VSMOW2-SLAP2 scale, we measured common silicate standards: San Carlos Olivine, NBS28, NMQ, and SKFS that have been calibrated to VSMOW2-SLAP2. Our reported Δ′<sup>17</sup>O error for silver phosphate is 10 per meg, calculated using the average long-term standard deviation of our two most replicated standards.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>We report the δ<sup>17</sup>O, δ<sup>18</sup>O, and Δ′<sup>17</sup>O values for a large suite of silver phosphate standards and present two new standards that can be used for interlaboratory calibration. Our results are reported on the VSMOW2-SLAP2 scale by measuring silicates on the same instrument with the same reference gas. The fluorination method in nickel reaction vessels is easily adapted to other laboratories that have fluorination lines. Only 2–3 mg of silver phosphate is needed for Δ′<sup>17</sup>O measurements when paired with δ<sup>18</sup>O values using the TC-EA technique.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"40 7","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://analyticalsciencejournals.onlinelibrary.wiley.com/doi/epdf/10.1002/rcm.70016","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145970070","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Charmatography based pphytochemical extraction to identify and quantification of volatile bioactive compounds providing chemical profiling to evaluate their pharmacological significance.
Methods
The component composition of essential oils of Bilacunaria microcarpa (M. Bieb.) Pimenov & V.N.Tikhom. and Peucedanum ruthenicum M. Bieb. distributed in the flora of Azerbaijan was studied using the method of gas chromatography–mass spectroscopy.
Results
In the composition of the essential oil of B. microcarpa, 70 components were found, of which 59 were identified; the mains of them are beta-phellandrene (12.86%), beta-pinene (10.18%), O-cymol (8.84%), L-borneol (7.85%), 1R-alpha-pinene (7.64%), caryophyllene (7.37%), beta-caryophyllene oxide (4.43%), and β-elemene (3.97%). In the essential oil of P. ruthenicum that were also identified, 60 of them were major components, of which are m-cymene (14.08%), beta-myrcene (13.34%), limonene (9.01%), 2-methylenebornane (6.68%), acetylcyclopentanone (4.39%), 1R-alpha-pinene (3.90%), and cryptone (3.77%). Antifungal activity of both B. microcarpa and P. ruthenicum species, as well as their aqueous extracts and essential oils, was revealed.
Conclusions
It was found that the studied plants and their aqueous extracts exhibit fungistatic activity on the growth of Trichoderma lignorum and Aspergillus niger fungal colonies, whereas B. microcarpa and their aqueous extracts exhibit fungicidal action on Fusarium oxysporum, and essential oils of the studied species in all concentrations exhibited absolute fungicidal action against this fungus, Aspergillus niger.
{"title":"Methodological Advances in GC–MS for Complex Plant Matrices: Profiling Essential Oils From Apiaceae Flora","authors":"Naiba Mehdiyeva, Nigar Mursal, Muhammad Zafar, Salman Majeed, Modhi O. Alotaibi, Khuzin Dinislam, Murodjon Yaxshimuratov, Mukhayya Ruzieva, Hami Halima, Enkelejda Kucaj","doi":"10.1002/rcm.70029","DOIUrl":"10.1002/rcm.70029","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>Charmatography based pphytochemical extraction to identify and quantification of volatile bioactive compounds providing chemical profiling to evaluate their pharmacological significance.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>The component composition of essential oils of <i>Bilacunaria microcarpa</i> (M. Bieb.) Pimenov & V.N.Tikhom. and <i>Peucedanum ruthenicum</i> M. Bieb. distributed in the flora of Azerbaijan was studied using the method of gas chromatography–mass spectroscopy.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>In the composition of the essential oil of <i>B. microcarpa</i>, 70 components were found, of which 59 were identified; the mains of them are beta-phellandrene (12.86%), beta-pinene (10.18%), O-cymol (8.84%), L-borneol (7.85%), 1R-alpha-pinene (7.64%), caryophyllene (7.37%), beta-caryophyllene oxide (4.43%), and β-elemene (3.97%). In the essential oil of <i>P. ruthenicum</i> that were also identified, 60 of them were major components, of which are m-cymene (14.08%), beta-myrcene (13.34%), limonene (9.01%), 2-methylenebornane (6.68%), acetylcyclopentanone (4.39%), 1R-alpha-pinene (3.90%), and cryptone (3.77%). Antifungal activity of both <i>B. microcarpa</i> and <i>P. ruthenicum</i> species, as well as their aqueous extracts and essential oils, was revealed.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>It was found that the studied plants and their aqueous extracts exhibit fungistatic activity on the growth of <i>Trichoderma lignorum</i> and <i>Aspergillus niger</i> fungal colonies, whereas <i>B. microcarpa</i> and their aqueous extracts exhibit fungicidal action on <i>Fusarium oxysporum</i>, and essential oils of the studied species in all concentrations exhibited absolute fungicidal action against this fungus, <i>Aspergillus niger</i>.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"40 7","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145984302","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Luan Felipe Campos Oliveira, Jose Javier Melendez-Perez, Sérgio Eduardo Bernardo Mistura Lutzer, Alessandra Sussulini, Marcos Nogueira Eberlin
Rationale
Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) is the gold standard in MS petroleomics due to its ultrahigh resolution and mass accuracy. But its high acquisition and maintenance costs limit accessibility. High-field Orbitrap (HFO) mass spectrometry is emerging as a promising alternative, but further evaluation is needed to determine its effectiveness in key analytical challenges of petroleomics, such as the molecular characterization of crude oils from different geological origins.
Methods
Ten crude oil samples from the Brazilian pre-salt region (five each of marine and lacustrine origin from two distinct sedimentary basins) were analyzed using ESI(−) FT-ICR MS and ESI(−) HFO MS (resolution: 840 000 at m/z 400). Molecular formula assignments were classified into heteroatom groups (NSO), and the data were interpreted using box plots, DBE vs. carbon number diagrams, and principal component analysis.
Results
HFO assigned ca. 2500 molecular formulae, compared to ca. 4500 assigned by FT-ICR. Despite this 45% lower performance, HFO preserved the overall profile of the major heteroatom classes. Notably, S1O4-containing compounds, which are critical markers, were identified at higher abundances with HFO, whereas marine and lacustrine oils were successfully discriminated based on NSO profiles, DBE, and carbon number. Marine oils exhibited higher oxygen content, DBE, and carbon number, whereas lacustrine oils showed relatively higher nitrogen content.
Conclusions
Despite reduced performance in formula assignments as compared to FT-ICR, HFO successfully distinguished crude oils of different geochemical origins. The present results indicate therefore that HFO, although displaying inferior performance than FT-ICR, particularly above m/z 400, still displays good enough mass resolution and accuracy sufficient to provide high quality petroleomic data normally required in most, if not all, common MS petroleomic investigations.
{"title":"Petroleomic by Mass Spectrometry of Geochemical Biomarkers of Polar and Nonvolatile Crude Oil Fractions: Fourier Transform Ion Cyclotron Resonance Versus High-Field Orbitrap","authors":"Luan Felipe Campos Oliveira, Jose Javier Melendez-Perez, Sérgio Eduardo Bernardo Mistura Lutzer, Alessandra Sussulini, Marcos Nogueira Eberlin","doi":"10.1002/rcm.70024","DOIUrl":"10.1002/rcm.70024","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) is the gold standard in MS petroleomics due to its ultrahigh resolution and mass accuracy. But its high acquisition and maintenance costs limit accessibility. High-field Orbitrap (HFO) mass spectrometry is emerging as a promising alternative, but further evaluation is needed to determine its effectiveness in key analytical challenges of petroleomics, such as the molecular characterization of crude oils from different geological origins.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>Ten crude oil samples from the Brazilian pre-salt region (five each of marine and lacustrine origin from two distinct sedimentary basins) were analyzed using ESI(−) FT-ICR MS and ESI(−) HFO MS (resolution: 840 000 at <i>m/z</i> 400). Molecular formula assignments were classified into heteroatom groups (NSO), and the data were interpreted using box plots, DBE vs. carbon number diagrams, and principal component analysis.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>HFO assigned ca. 2500 molecular formulae, compared to ca. 4500 assigned by FT-ICR. Despite this 45% lower performance, HFO preserved the overall profile of the major heteroatom classes. Notably, S<sub>1</sub>O<sub>4</sub>-containing compounds, which are critical markers, were identified at higher abundances with HFO, whereas marine and lacustrine oils were successfully discriminated based on NSO profiles, DBE, and carbon number. Marine oils exhibited higher oxygen content, DBE, and carbon number, whereas lacustrine oils showed relatively higher nitrogen content.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>Despite reduced performance in formula assignments as compared to FT-ICR, HFO successfully distinguished crude oils of different geochemical origins. The present results indicate therefore that HFO, although displaying inferior performance than FT-ICR, particularly above <i>m/z</i> 400, still displays good enough mass resolution and accuracy sufficient to provide high quality petroleomic data normally required in most, if not all, common MS petroleomic investigations.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"40 6","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-01-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145905374","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Heyi Xu, You Jiang, Jie Xie, Li Yao, Xiang Fang, Meiying Liu, Ziyu Qu, Guang Yang, Di Zhang
Rationale
Dissociation is a critical analytical method in mass spectrometry research. Among various dissociation techniques, higher energy collision dissociation (HCD) stands out as a pivotal tool due to its ability to generate more low-mass fragment ions and directly perform dissociation during mass spectrometric detection. However, existing HCD implementations rely on specialized instrument configurations, such as collision cell structures or triple quadrupole mass spectrometers, which inevitably increase instrument development costs and technical complexity. To address this limitation, this study proposes an HCD method based on dual-pressure linear ion trap mass spectrometry that requires no additional hardware modifications.
Methods
Instead, it achieves HCD solely by optimizing the instrument's gas flow system and control parameters. By employing a nitrogen-helium gas mixture as the collision gas and testing with a reserpine standard sample, optimal dissociation conditions were obtained through adjustments to the gas mixture ratio and ion trap DC offset voltage settings.
Results
This approach successfully realizes in-trap HCD directly within the dual-pressure linear ion trap, eliminating the need for a dedicated collision cell. Furthermore, it enables HCD-based MS3 functionality, a capability unavailable in traditional triple quadrupole systems.
Conclusions
Validation experiments using veterinary drug residues fenoterol and ractopamine demonstrated the method's universality by comparing its dissociation results with those from conventional ion trap collision-induced dissociation (CID) and triple quadrupole method. The findings confirm that this strategy can be extended to other ion trap mass spectrometry platforms, offering broader applicability.
{"title":"Investigation of In-Trap High-Energy Collision Dissociation Methodology and Dissociation Conditions Using Dual-Pressure Linear Ion Trap Mass Spectrometry","authors":"Heyi Xu, You Jiang, Jie Xie, Li Yao, Xiang Fang, Meiying Liu, Ziyu Qu, Guang Yang, Di Zhang","doi":"10.1002/rcm.70025","DOIUrl":"10.1002/rcm.70025","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>Dissociation is a critical analytical method in mass spectrometry research. Among various dissociation techniques, higher energy collision dissociation (HCD) stands out as a pivotal tool due to its ability to generate more low-mass fragment ions and directly perform dissociation during mass spectrometric detection. However, existing HCD implementations rely on specialized instrument configurations, such as collision cell structures or triple quadrupole mass spectrometers, which inevitably increase instrument development costs and technical complexity. To address this limitation, this study proposes an HCD method based on dual-pressure linear ion trap mass spectrometry that requires no additional hardware modifications.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>Instead, it achieves HCD solely by optimizing the instrument's gas flow system and control parameters. By employing a nitrogen-helium gas mixture as the collision gas and testing with a reserpine standard sample, optimal dissociation conditions were obtained through adjustments to the gas mixture ratio and ion trap DC offset voltage settings.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>This approach successfully realizes in-trap HCD directly within the dual-pressure linear ion trap, eliminating the need for a dedicated collision cell. Furthermore, it enables HCD-based MS3 functionality, a capability unavailable in traditional triple quadrupole systems.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>Validation experiments using veterinary drug residues fenoterol and ractopamine demonstrated the method's universality by comparing its dissociation results with those from conventional ion trap collision-induced dissociation (CID) and triple quadrupole method. The findings confirm that this strategy can be extended to other ion trap mass spectrometry platforms, offering broader applicability.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"40 6","pages":""},"PeriodicalIF":1.7,"publicationDate":"2026-01-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145905377","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Chemicals migrating from plastic and take-out food packaging can leach into food, posing inherent health risks to consumers. Given the ubiquitous use of plastic packaging in daily diets, reliable analytical methods for detecting restricted substances in food contact materials are imperative for safeguarding public health.
Methods
A novel analytical method, coupling gas chromatography–mass spectrometry (GC–MS) with liquid–liquid extraction for sample pretreatment, was established for the simultaneous separation and quantification of 15 common restricted substances (10 plasticizers, 1 antioxidant, and 4 ultraviolet absorbers) migrating from food plastic packaging materials into food products.
Results
The method exhibited excellent linearity (correlation coefficients, r > 0.99) across wide concentration ranges, with limits of detection (LODs) ranging from 0.005 to 0.046 mg/L. Validation data showed average recoveries of 72.30%–109.03% and relative standard deviations (RSDs, n = 6) of 1.13%–26.50%, confirming its analytical reliability.
Conclusions
This method enables rapid and accurate determination of the 15 target restricted substances, facilitating migration monitoring in food plastic packaging and strengthening technical support for food safety assessment in daily and take-out food contexts.
{"title":"Determination of 15 Restricted Substances in Plastic-Packaged Food by Gas Chromatography–Mass Spectrometry","authors":"Xin Yang, Hanning Zhang, Jinqiang Yan, Hongmei Xue, Hongmei Shi, Junjie Miao","doi":"10.1002/rcm.70023","DOIUrl":"10.1002/rcm.70023","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>Chemicals migrating from plastic and take-out food packaging can leach into food, posing inherent health risks to consumers. Given the ubiquitous use of plastic packaging in daily diets, reliable analytical methods for detecting restricted substances in food contact materials are imperative for safeguarding public health.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>A novel analytical method, coupling gas chromatography–mass spectrometry (GC–MS) with liquid–liquid extraction for sample pretreatment, was established for the simultaneous separation and quantification of 15 common restricted substances (10 plasticizers, 1 antioxidant, and 4 ultraviolet absorbers) migrating from food plastic packaging materials into food products.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>The method exhibited excellent linearity (correlation coefficients, <i>r</i> > 0.99) across wide concentration ranges, with limits of detection (LODs) ranging from 0.005 to 0.046 mg/L. Validation data showed average recoveries of 72.30%–109.03% and relative standard deviations (RSDs, <i>n</i> = 6) of 1.13%–26.50%, confirming its analytical reliability.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>This method enables rapid and accurate determination of the 15 target restricted substances, facilitating migration monitoring in food plastic packaging and strengthening technical support for food safety assessment in daily and take-out food contexts.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"40 6","pages":""},"PeriodicalIF":1.7,"publicationDate":"2025-12-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145852726","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Maximilian Hansen, Jakob Brettschneider, Hubert Vonhof, Denis Scholz
Rationale
The Delta Ray Isotope Ratio Infrared Spectrometer enables to determine δ13C and δ18O values of CO2. The measurements are calibrated against internal reference gas standards. For discrete carbonate or dissolved inorganic carbon (DIC) samples, the manufacturer recommends a calibration against two isotopically different carbonate standard materials (i.e., a 2-point calibration). Here, we show that this method is not sufficient because the measured values may drift significantly over the duration of a measurement run (i.e., 58 samples in approximately 24 h).
Methods
We developed a new measurement routine applying a 3-point calibration and a tight standard-bracketing. In addition, we present an R code to automatically evaluate and calibrate the measured data.
Results
Our standard-bracketing technique can effectively correct drifts of more than 1‰ not accounted for by the internally calibrated data. A 3-point calibration with four samples bracketed by two sets of standards provides the highest precision and accuracy, that is, the highest reproducibility for our carbonate samples. The third standard stabilizes the calibration curve and enables to better identify individual outliers.
Conclusions
Our standard-bracketing method enables accurate and precise (< 0.1‰) measurements of δ13C and δ18O values of calcite and DIC using the Delta Ray IRIS over a large range of values (ranging from approximately −37‰ to +2‰ in δ13C and from approximately −25‰ to −2‰ in δ18O).
{"title":"Stable Carbon and Oxygen Isotope Analysis of Carbonates and DIC Using the Delta Ray Isotope Ratio Infrared Spectrometer (IRIS): Precise and Accurate Measurements Applying a 3-Point Calibration and Standard Bracketing","authors":"Maximilian Hansen, Jakob Brettschneider, Hubert Vonhof, Denis Scholz","doi":"10.1002/rcm.70021","DOIUrl":"10.1002/rcm.70021","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>The Delta Ray Isotope Ratio Infrared Spectrometer enables to determine δ<sup>13</sup>C and δ<sup>18</sup>O values of CO<sub>2</sub>. The measurements are calibrated against internal reference gas standards. For discrete carbonate or dissolved inorganic carbon (DIC) samples, the manufacturer recommends a calibration against two isotopically different carbonate standard materials (i.e., a 2-point calibration). Here, we show that this method is not sufficient because the measured values may drift significantly over the duration of a measurement run (i.e., 58 samples in approximately 24 h).</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>We developed a new measurement routine applying a 3-point calibration and a tight standard-bracketing. In addition, we present an R code to automatically evaluate and calibrate the measured data.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>Our standard-bracketing technique can effectively correct drifts of more than 1‰ not accounted for by the internally calibrated data. A 3-point calibration with four samples bracketed by two sets of standards provides the highest precision and accuracy, that is, the highest reproducibility for our carbonate samples. The third standard stabilizes the calibration curve and enables to better identify individual outliers.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>Our standard-bracketing method enables accurate and precise (< 0.1‰) measurements of δ<sup>13</sup>C and δ<sup>18</sup>O values of calcite and DIC using the Delta Ray IRIS over a large range of values (ranging from approximately −37‰ to +2‰ in δ<sup>13</sup>C and from approximately −25‰ to −2‰ in δ<sup>18</sup>O).</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"40 6","pages":""},"PeriodicalIF":1.7,"publicationDate":"2025-12-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12748363/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145852664","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Zircon Zr isotopic variations hold great potential for tracing magmatic crystallization and differentiation processes, although the mechanisms of Zr isotopic fractionation remain highly debated. High spatial resolution, nearly non-destructive Zr isotopic analysis of zircon, allows for a more detailed investigation of Zr isotopic variations in structurally complex or tiny zircons.
Methods
This study systematically optimized key parameters (e.g., primary beam current, beam diameter, raster size,and signal acquisition time) and further evaluated the topography effect using dynamic transfer parameters, ultimately establishing a high spatial resolution secondary ion mass spectrometry (SIMS) method for zircon Zr isotope microanalysis.
Results
The internal precision (twice the standard error [2SE]) for δ94Zr measurements in zircon reference materials (i.e., Mudtank, Penglai, Plešovice, Tanz) ranged from 0.07‰ to 0.16‰, with external reproducibility better than 0.15‰ (twice the standard deviation [2SD]). The Zr isotopic compositions of reference materials measured by SIMS agree remarkably well with the recommended values by double-spike solution methods. Our method consumes ~0.05 ng of mineral material in a single spot analysis with a high spatial resolution of ~10 × 9 μm2 and a pit depth of ~0.5 μm.
Conclusions
This nearly nondestructive technique is suitable for analyzing structurally complex or precious samples, such as zircon from lunar soil, advancing the study of magmatic processes.
{"title":"High Spatial Resolution (< 10 μm) Zircon SIMS Zr Isotope Analysis","authors":"Sheng He, Yang Li, Liguang Wu, Xianhua Li","doi":"10.1002/rcm.70020","DOIUrl":"10.1002/rcm.70020","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p>Zircon Zr isotopic variations hold great potential for tracing magmatic crystallization and differentiation processes, although the mechanisms of Zr isotopic fractionation remain highly debated. High spatial resolution, nearly non-destructive Zr isotopic analysis of zircon, allows for a more detailed investigation of Zr isotopic variations in structurally complex or tiny zircons.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>This study systematically optimized key parameters (e.g., primary beam current, beam diameter, raster size,and signal acquisition time) and further evaluated the topography effect using dynamic transfer parameters, ultimately establishing a high spatial resolution secondary ion mass spectrometry (SIMS) method for zircon Zr isotope microanalysis.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>The internal precision (twice the standard error [2SE]) for δ<sup>94</sup>Zr measurements in zircon reference materials (i.e., Mudtank, Penglai, Plešovice, Tanz) ranged from 0.07‰ to 0.16‰, with external reproducibility better than 0.15‰ (twice the standard deviation [2SD]). The Zr isotopic compositions of reference materials measured by SIMS agree remarkably well with the recommended values by double-spike solution methods. Our method consumes ~0.05 ng of mineral material in a single spot analysis with a high spatial resolution of ~10 × 9 μm<sup>2</sup> and a pit depth of ~0.5 μm.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>This nearly nondestructive technique is suitable for analyzing structurally complex or precious samples, such as zircon from lunar soil, advancing the study of magmatic processes.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"40 6","pages":""},"PeriodicalIF":1.7,"publicationDate":"2025-12-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145809113","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Marco Rolando Aronés Jara, Rosy Yesela Mancilla Santa Cruz, Kirianova Godoy Bautista, Edgar Cárdenas Landeo, Edith Eveling Conislla Cáceres, Hugo Roberto Luna Molero, Juan Clímaco Paniagua Segovia, Anas Rashid, María Segunda Aurora Prado
Rationale
Niphidium crassifolium (Linnaeus) Lellinger is a fern from the Polypodiaceae family, native to Central and South America, with traditional uses in herbal medicine. Despite its recognized ethnomedical value, its phytochemical composition has not been extensively studied. This pioneering work aimed to determine the metabolite profile from rhizomes of N. crassifolium, to quantify the contents of phenols and flavonoids, and to evaluate their antioxidant and antibacterial activities.
Methods
Metabolite characterization was performed using LC-MS/MS, while radical scavenging activity (DPPH• and ABTS•+ assays) was used to estimate in vitro antioxidant potential. Trolox was used as reference standard in both assays. Phenolic and flavonoid contents as well as antioxidant activity were evaluated in four anatomical parts: complete rhizome, proximal rhizome, distal rhizome, and adventitious root.
Results
This study identified the presence of saponins, phytoecdysteroids, flavones, phenolic acids, and phenolic glycosides. Proximal rhizome exhibited the highest phenolic content (264.6 ± 0.15 mg GAE/g), whereas adventitious root showed the highest flavonoid content (54.0 ± 0.47 mg RUE/g). Median effective concentration of proximal rhizome was 50.4 ± 0.03 μg/mL (DPPH•) and 310.7 ± 1.9 μg/mL (ABTS•+), compared to Trolox values of 37.4 ± 0.01 μg/mL and 155.0 ± 0.3 μg/mL, respectively (p < 0.05). Despite slightly higher EC50 values than Trolox, proximal rhizome's antioxidant capacity was statistically significant (p < 0.05). Plant exhibited selective antibacterial activity against Gram-positive bacteria, particularly Staphylococcus aureus ATCC 6538 (inhibition halo, 16.5 ± 0.09 mm; minimum inhibitory concentration, 13 370 μg/mL) and Bacillus spizizenii ATCC 6633 (inhibition halo, 12.6 ± 0.40 mm; minimum inhibitory concentration, 3 230 μg/mL).
Conclusions
These findings underscore the value of N. crassifolium as a promising source of antioxidant and antibacterial compounds. Data support its ethnomedical applications and underscore the potential for development into natural therapeutic agents targeting oxidative stress and Gram-positive infections that pave the way for future pharmaceutical and nutraceutical development.
{"title":"UHPLC-MS/MS Comprehensive Phytochemical Investigation of Niphidium crassifolium Rhizome: Bioactivity Assessment With Insights Into In Vitro Antioxidant and Antibacterial Potentials","authors":"Marco Rolando Aronés Jara, Rosy Yesela Mancilla Santa Cruz, Kirianova Godoy Bautista, Edgar Cárdenas Landeo, Edith Eveling Conislla Cáceres, Hugo Roberto Luna Molero, Juan Clímaco Paniagua Segovia, Anas Rashid, María Segunda Aurora Prado","doi":"10.1002/rcm.70014","DOIUrl":"10.1002/rcm.70014","url":null,"abstract":"<div>\u0000 \u0000 \u0000 <section>\u0000 \u0000 <h3> Rationale</h3>\u0000 \u0000 <p><i>Niphidium crassifolium</i> (Linnaeus) Lellinger is a fern from the <i>Polypodiaceae</i> family, native to Central and South America, with traditional uses in herbal medicine. Despite its recognized ethnomedical value, its phytochemical composition has not been extensively studied. This pioneering work aimed to determine the metabolite profile from rhizomes of <i>N. crassifolium</i>, to quantify the contents of phenols and flavonoids, and to evaluate their antioxidant and antibacterial activities.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Methods</h3>\u0000 \u0000 <p>Metabolite characterization was performed using LC-MS/MS, while radical scavenging activity (DPPH<sup>•</sup> and ABTS<sup>•+</sup> assays) was used to estimate in vitro antioxidant potential. Trolox was used as reference standard in both assays. Phenolic and flavonoid contents as well as antioxidant activity were evaluated in four anatomical parts: complete rhizome, proximal rhizome, distal rhizome, and adventitious root.</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Results</h3>\u0000 \u0000 <p>This study identified the presence of saponins, phytoecdysteroids, flavones, phenolic acids, and phenolic glycosides. Proximal rhizome exhibited the highest phenolic content (264.6 ± 0.15 mg GAE/g), whereas adventitious root showed the highest flavonoid content (54.0 ± 0.47 mg RUE/g). Median effective concentration of proximal rhizome was 50.4 ± 0.03 μg/mL (DPPH<sup>•</sup>) and 310.7 ± 1.9 μg/mL (ABTS<sup>•+</sup>), compared to Trolox values of 37.4 ± 0.01 μg/mL and 155.0 ± 0.3 μg/mL, respectively (<i>p</i> < 0.05). Despite slightly higher EC<sub>50</sub> values than Trolox, proximal rhizome's antioxidant capacity was statistically significant (<i>p</i> < 0.05). Plant exhibited selective antibacterial activity against Gram-positive bacteria, particularly <i>Staphylococcus aureus</i> ATCC 6538 (inhibition halo, 16.5 ± 0.09 mm; minimum inhibitory concentration, 13 370 μg/mL) and <i>Bacillus spizizenii</i> ATCC 6633 (inhibition halo, 12.6 ± 0.40 mm; minimum inhibitory concentration, 3 230 μg/mL).</p>\u0000 </section>\u0000 \u0000 <section>\u0000 \u0000 <h3> Conclusions</h3>\u0000 \u0000 <p>These findings underscore the value of <i>N. crassifolium</i> as a promising source of antioxidant and antibacterial compounds. Data support its ethnomedical applications and underscore the potential for development into natural therapeutic agents targeting oxidative stress and Gram-positive infections that pave the way for future pharmaceutical and nutraceutical development.</p>\u0000 </section>\u0000 </div>","PeriodicalId":225,"journal":{"name":"Rapid Communications in Mass Spectrometry","volume":"40 6","pages":""},"PeriodicalIF":1.7,"publicationDate":"2025-12-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145809266","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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