March 18th, 2015
The results and winners of CASMI-2014 are now up. March 3rd, 2015
The solutions for CASMI-2014 are now available on the website. January 15th, 2015
The CASMI 2014 Challenges submissions deadline has been extended to February 15th, 2015! September 15th, 2014
The CASMI 2014 Challenges are now officially available ! September 2nd, 2014
All articles of the CASMI 2013 proceedings are now online. April 30, 2014
First announcement at the Analytical Tools for Cutting-edge Metabolomics meeting.
Challenge 1
This molecule was detected in human cardiac tissue with a retention time of 5.52 minutes. The data were acquired applying UPLC-MS on a Waters ACQUITY UPLC integrated with a Thermo Scientific Orbitrap Velos mass spectrometer operating in electrospray positive ion mode. A Waters ACQUITY UPLC BEH C18 (2.1 mm × 100 mm, 1.7 µm) column was applied. A reversed phase linear gradient elution operating at a flow rate of 0.40mL/min over 15 minutes from 95%A to 5%A was applied with water (+0.1% formic acid) as solvent A and methanol (+0.1% formic acid) as solvent B. The expected mass accuracy of the instrument is <3ppm. MS/MS data were acquired in positive ion mode applying HCD and m/z measurements in the Orbitrap Velos with a precursor selection width of +/-1.5Da, m/z range > 100, a precursor m/z of 480 and normalised collision energy of 25%. The expected mass accuracy for MS/MS data is <5ppm.
Challenge 2
This molecule was detected in a human endothelial cell extract with a retention time of 267 seconds. The data were acquired applying UPLC-MS on a Thermo Scientific Accela integrated with a Thermo Scientific Orbitrap Velos mass spectrometer operating in electrospray positive ion mode. A Waters ACQUITY UPLC BEH C18 (2.1 mm × 100 mm, 1.7 µm) column was applied. A reversed phase linear gradient elution operating at a flow rate of 0.35mL/min over 18 minutes from 95%A to 5%A was applied with water (+0.1% formic acid) as solvent A and methanol (+0.1% formic acid) as solvent B. The expected mass accuracy of the instrument is <5ppm. MS/MS data were acquired in positive ion mode applying HCD and m/z measurements in the Orbitrap Velos with a precursor selection width of +/-1.5Da, m/z range > 100, a precursor m/z of 206 and normalised collision energy of 40%. The expected mass accuracy for MS/MS data is <5ppm.
Challenge 3
This molecule was detected in human urine with a retention time of 3.38 minutes. The data were acquired applying UPLC-MS on a Thermo Scientific Ultimate3000 integrated with a Thermo Scientific Q Exactive mass spectrometer operating in electrospray negative ion mode. A Thermo Scientific Accucore Amide HILIC (2.1 mm × 100 mm, 2.6µm) column was applied. A HILIC linear gradient elution operating at a flow rate of 0.20mL/min over 12 minutes was applied from 5%B to 50%B with acetonitrile (with 5mM ammonium acetate) as solvent A and water (with 5mM ammonium acetate) as solvent B. The expected mass accuracy of the instrument is <3ppm. MS/MS data were acquired in negative ion mode applying HCD and m/z measurements in the Q Exactive with a precursor selection width of +/-1.5Da, a precursor m/z of 194 and normalised collision energy of 80%. The expected mass accuracy for MS/MS data is <5ppm.
Challenge 4
This molecule was detected in human CSF with a retention time of 154 seconds. The data were acquired applying UPLC-MS on a Waters Acquity UPLC integrated with a Thermo Scientific Orbitrap Velos mass spectrometer operating in electrospray negative ion mode. A Waters ACQUITY UPLC BEH C18 (2.1 mm × 100 mm, 1.7 µm) column was applied. A reversed phase linear gradient elution operating at a flow rate of 0.35 mL/min over 10 minutes from 95%A to 5%A was applied with water (+0.1% formic acid) as solvent A and methanol (+0.1% formic acid) as solvent B. The expected mass accuracy of the instrument is <5ppm. MS/MS data were acquired in negative ion mode applying CID in the linear ion trap and m/z measurements in the Orbitrap Velos with a precursor selection width of +/-1.5Da, m/z range > 100, a precursor m/z of 225 and normalised collision energy of 30%. The expected mass accuracy for MS/MS data is <5ppm.
Challenge 5
This molecule was detected in human serum with a retention time of 184 seconds. The data were acquired applying UPLC-MS on a Thermo Scientific Ultimate3000 integrated with a Thermo Scientific Q Exactive mass spectrometer operating in electrospray negative ion mode. A Thermo Scientific GOLD C18 (2.1 mm × 100 mm, 1.9µm) column was applied. A reversed phase linear gradient elution operating at a flow rate of 0.35mL/min over 12 minutes from 95%A to 5%A was applied with water (+0.1% formic acid) as solvent A and methanol (+0.1% formic acid) as solvent B. The expected mass accuracy of the instrument is <3ppm. MS/MS data were acquired in negative ion mode applying HCD and m/z measurements in the Q Exactive with a precursor selection width of +/-1.5Da, m/z range > 100, a precursor m/z of 219 and normalised collision energy of 80%. The expected mass accuracy for MS/MS data is <5ppm.
Challenge 6
This molecule was detected in human urine with a retention time of 209 seconds. The data were acquired applying UPLC-MS on a Thermo Scientific Ultimate3000 integrated with a Thermo Scientific Orbitrap Velos mass spectrometer operating in electrospray negative ion mode. A Thermo Scientific GOLD C18 (2.1 mm × 100 mm, 1.9µm) column was applied. A reversed phase linear gradient elution operating at a flow rate of 0.35mL/min over 10 minutes from 95%A to 5%A was applied with water (+0.1% formic acid) as solvent A and methanol (+0.1% formic acid) as solvent B. The expected mass accuracy of the instrument is <5ppm. MS/MS data were acquired in negative ion mode applying HCD and m/z measurements in the Orbitrap Velos with a precursor selection width of +/-1.5Da, m/z range > 100, a precursor m/z of 167 and normalised collision energy of 70%. The expected mass accuracy for MS/MS data is <5ppm.
Challenge 7
This molecule was detected in human plasma with a retention time of 493 seconds. The data were acquired applying UPLC-MS on a Waters Acquity UPLC integrated with a Thermo Scientific Orbitrap Velos mass spectrometer operating in electrospray positive ion mode. A Waters ACQUITY UPLC BEH C18 (2.1 mm × 100 mm, 1.7 µm) column was applied. A reversed phase linear gradient elution operating at a flow rate of 0.35mL/min over 15 minutes from 95%A to 5%A was applied with water (+0.1% formic acid) as solvent A and methanol (+0.1% formic acid) as solvent B. The expected mass accuracy of the instrument is <3ppm. MS/MS data were acquired in positive ion mode applying HCD and m/z measurements in the Orbitrap Velos with a precursor selection width of +/-1.5Da, a precursor m/z of 385 and normalised collision energy of 30%. The expected mass accuracy for MS/MS data is <5ppm.
Challenge 8
This molecule was detected in human serum with a retention time of 65 seconds. The data were acquired applying UPLC-MS on a Thermo Scientific Ultimate3000 integrated with a Thermo Scientific Q Exactive mass spectrometer operating in electrospray positive ion mode. A Thermo Scientific GOLD C18 (2.1 mm × 100 mm, 1.9µm) column was applied. A reversed phase linear gradient elution operating at a flow rate of 0.35mL/min over 10 minutes from 95%A to 5%A was applied with water (+0.1% formic acid) as solvent A and methanol (+0.1% formic acid) as solvent B. The expected mass accuracy of the instrument is <5ppm. MS/MS data were acquired in positive ion mode applying HCD and m/z measurements in the Q Exactive with a precursor selection width of +/-1.5Da, m/z range > 100, a precursor m/z of 365 and normalised collision energy of 40%. The expected mass accuracy for MS/MS data is <5ppm.
Challenge 9
This molecule was detected in human urine with a retention time of 5.40 minutes. The data were acquired applying UPLC-MS on a Thermo Scientific Accela integrated with a Thermo Scientific Orbitrap Velos mass spectrometer operating in electrospray positive ion mode. A Thermo Scientific Accucore Amide HILIC (2.1 mm × 100 mm, 2.6µm) column was applied. A HILIC linear gradient elution operating at a flow rate of 0.20mL/min over 12 minutes was applied from 5%B to 50%B with acetonitrile (with 5mM ammonium acetate) as solvent A and water (with 5mM ammonium acetate) as solvent B. The expected mass accuracy of the instrument is <5ppm. MS/MS data were acquired in positive ion mode applying CID in the linear ion trap and m/z measurements in the Orbitrap Velos with a precursor selection width of +/-1.5Da, m/z range > 100, a precursor m/z of 308 and normalised collision energy of 35%. The expected mass accuracy for MS/MS data is <5ppm.
Challenge 10
This molecule was detected in human urine with a retention time of 3.56 minutes. The data were acquired applying UPLC-MS on a Thermo Scientific Accela integrated with a Thermo Scientific Orbitrap Velos mass spectrometer operating in electrospray positive ion mode. A Thermo Scientific Accucore Amide HILIC (2.1 mm × 100 mm, 2.6µm) column was applied. A HILIC linear gradient elution operating at a flow rate of 0.40mL/min over 12 minutes was applied from 5%B to 50%B with acetonitrile (with 5mM ammonium acetate) as solvent A and water (with 5mM ammonium acetate) as solvent B. The expected mass accuracy of the instrument is <5ppm. MS/MS data were acquired in positive ion mode applying HCD and m/z measurements in the Orbitrap Velos with a precursor selection width of +/-1.5Da, a precursor m/z of 348 and normalised collision energy of 60%. The expected mass accuracy for MS/MS data is <5ppm.
Challenge 11
This molecule was detected in human serum with a retention time of 174 seconds. The data were acquired applying UPLC-MS on a Thermo Scientific Ultimate3000 UPLC integrated with a Thermo Scientific Q Exactive mass spectrometer operating in electrospray positive ion mode. A Thermo Scientific GOLD C18 (2.1 mm × 100 mm, 1.9µm) column was applied. A reversed phase linear gradient elution operating at a flow rate of 0.35mL/min over 10 minutes from 95%A to 5%A was applied with water (+0.1% formic acid) as solvent A and methanol (+0.1% formic acid) as solvent B. The expected mass accuracy of the instrument is <3ppm. MS/MS data were acquired in positive ion mode applying HCD and m/z measurements in the Q Exactive with a precursor selection width of +/-1.5Da, m/z range > 100, a precursor m/z of 181 and normalised collision energy of 90%. The expected mass accuracy for MS/MS data is <5ppm.
Challenge 12
This molecule was detected in human tissues. The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in positive ion electrospray mode. Reversed phase separation was carried out using a Waters XBridge 2.0 x 50mm C18 column (2.5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 20-95%B operating at a flow rate of 0.22mL/min over 10 minutes was applied. Under these conditions the compound eluted at the retention time of 0.8 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 205 and a collision energy of 10eV.
Challenge 13
This molecule was detected in human serum and tissues. The contest data were acquired on a Shimadzu Prominence UFLC XR solvent delivery system integrated with a Shimadzu LC-MS-IT-TOF ion trap/time-of flight (IT-TOF) mass spectrometer operating in negative ion electrospray mode. Reversed phase separation was carried out using a Waters XBridge 2.0 x 50mm C18 column (2.5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 20-95%B operating at a flow rate of 0.22mL/min over 10 minutes was applied. Under these conditions the compound eluted at the retention time of 6.1 min. The expected mass accuracy of the instrument is <7ppm. MS/MS data were collected under the following conditions: collision energy 50%, collision gas 50%; isolation width 1Da; activation q=0.25; ion accumulation ASC; precursor ion m/z 351; m/z range > 100.
Challenge 14
This molecule was detected in the human central nervous system. The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in positive ion electrospray mode. Reversed phase separation was carried out using a Hypersil GOLD 2.0 x 150mm C18 column (5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 6-36%B operating at a flow rate of 0.20mL/min over 30 minutes was applied. Under these conditions the compound eluted at the retention time of 2.8 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 224 and a collision energy of 15eV; m/z range > 100.
Challenge 15
This molecule has been detected in human urine and lens. The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in positive ion electrospray mode. Reversed phase separation was carried out using a Hypersil GOLD 2.0 x 150mm C18 column (5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 6-36%B operating at a flow rate of 0.20mL/min over 30 minutes was applied. Under these conditions the compound eluted at the retention time of 11.4 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 231 and a collision energy of 15eV; m/z range > 100.
Challenge 16
This molecule is an intermediate in the primary metabolism of many living organisms. The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in positive ion electrospray mode. Reversed phase separation was carried out using a Waters XBridge 2.0 x 50mm C18 column (2.5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 20-95%B operating at a flow rate of 0.22mL/min over 10 minutes was applied. Under these conditions the compound eluted at the retention time of 0.8 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 275 and a collision energy of 15eV.
Challenge 17
This molecule is a plant-derived product isolated from the Brassicacea family. The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in positive ion electrospray mode. Reversed phase separation was carried out using a Waters XBridge 2.0 x 50mm C18 column (2.5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 20-95%B operating at a flow rate of 0.22mL/min over 10 minutes was applied. Under these conditions the compound eluted at the retention time of 5.1 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 251 and a collision energy of 15eV.
Challenge 18
This molecule has been isolated from several plants, although it is considered by some as an isolation artifact. The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in positive ion electrospray mode. Reversed phase separation was carried out using a Waters XBridge 2.0 x 50mm C18 column (2.5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 20-95%B operating at a flow rate of 0.22mL/min over 10 minutes was applied. Under these conditions the compound eluted at the retention time of 1.0 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 253 and a collision energy of 15eV.
Challenge 19
This molecule is a plant-derived product isolated, among others, from the Compositae family. The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in positive ion electrospray mode. Reversed phase separation was carried out using a Waters XBridge 2.0 x 50mm C18 column (2.5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 5-50%B operating at a flow rate of 0.22mL/min over 10 minutes was applied. Under these conditions the compound eluted at the retention time of 6.3 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 366 and a collision energy of 25eV.
Challenge 20
This compound is a natural product isolated from Glycyrrhiza spp. The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in negative ion electrospray mode. Reversed phase separation was carried out using a Waters XBridge 2.0 x 50mm C18 column (2.5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 20-95%B operating at a flow rate of 0.22mL/min over 10 minutes was applied. Under these conditions the compound eluted at the retention time of 6.9 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 335 and a collision energy of 25eV.
Challenge 21
This compound is a natural product isolated from a terrestrial plant. The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in positive ion electrospray mode. Reversed phase separation was carried out using a Waters XBridge 2.0 x 50mm C18 column (2.5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 20-95%B operating at a flow rate of 0.22mL/min over 10 minutes was applied. Under these conditions the compound eluted at the retention time of 1.6 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 314 and a collision energy of 25eV.
Challenge 22
This compound is a natural product isolated from Trifolium spp. The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in positive ion electrospray mode. Reversed phase separation was carried out using a Waters XBridge 2.0 x 50mm C18 column (2.5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 20-85%B operating at a flow rate of 0.22mL/min over 10 minutes was applied. Under these conditions the compound eluted at the retention time of 6.6 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 285 and a collision energy of 15eV.
Challenge 23
This molecule is a bacterial product. The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in positive ion electrospray mode. Reversed phase separation was carried out using a Waters XBridge 2.0 x 50mm C18 column (2.5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 20-95%B operating at a flow rate of 0.22mL/min over 10 minutes was applied. Under these conditions the compound eluted at the retention time of 0.8 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 288 and a collision energy of 15eV.
Challenge 24
This molecule is a bacterial metabolite. The contest data were acquired on a Dionex solvent delivery system integrated with Thermo Fisher Scientific linear ion trap/FT-ICR (LTQ-FT Ultra) mass spectrometer operated in positive ion electrospray mode. The data were acquired using flow injection. The mobile phase consisted on 50:50 (v/v) water: acetonitrile both containing 0.1% formic acid. MS/MS data were acquired by applying CID in the linear ion trap (q=0.25 and activation time of 30 msec) and m/z measurements in the FT-ICR. For MS/MS, precursor selection width of +/-2.0Da was used, a precursor m/z of 478 for MS/MS and m/z 322 for MS3 data and a normalised collision energy of 35%. The FT-ICR was operated at the resolving power of 100,000. The expected mass accuracy for this instrument is <3ppm. A significant negative bias for the isotopic distribution is present in the data.
Challenge 25
MSMSThis molecule is a fungal metabolite. The contest data were acquired on a Dionex solvent delivery system integrated with Thermo Fisher Scientific linear ion trap/FT-ICR (LTQ-FT Ultra) mass spectrometer operated in negative ion electrospray mode. The data were acquired using flow injection. The mobile phase consisted on 50:50 (v/v) water: acetonitrile both containing 0.1% formic acid. MS/MS data were acquired by applying CID in the linear ion trap (q=0.25 and activation time of 30 msec) and m/z measurements in the FT-ICR. For MS/MS, precursor selection width of +/-2.0Da was used. Data are provided for both the precursor of m/z 515 and 561. Normalised collision energy of 35% was used for CID. The FT-ICR was operated at the resolving power of 100,000. The expected mass accuracy for this instrument is <3ppm. The isotopic peak for the ion of m/z 515 is not visible due to low abundance.
Challenge 26
This is molecule is a plant-derived natural product. The contest data were acquired on a Dionex solvent delivery system integrated with Thermo Fisher Scientific linear ion trap/FT-ICR (LTQ-FT Ultra) mass spectrometer operated in positive ion electrospray mode. The data were acquired using flow injection. The mobile phase consisted on 50:50 (v/v) water: acetonitrile both containing 0.1% formic acid. MS/MS data were acquired by applying CID in the linear ion trap (q=0.25 and activation time of 30 msec) and m/z measurements in the FT-ICR. For MS/MS, precursor selection width of +/-2.0Da was used, a precursor of m/z 503 and normalised collision energy of 35% was used. The FT-ICR was operated at the resolving power of 100,000. The expected mass accuracy for this instrument is <3ppm. Under the experimental conditions applied, no useful MS/MS spectrum was obtained for the precursor ion of m/z 463.
Challenge 27
This molecule is a plant-derived natural product. The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in positive ion electrospray mode. Reversed phase separation was carried out using a Waters XBridge 2.0 x 50mm C18 column (2.5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 20-95%B operating at a flow rate of 0.22mL/min over 10 minutes was applied. Under these conditions the compound eluted at the retention time of 3.6 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 351 and a collision energy of 6 eV.
Challenge 28
This molecule is a compound isolated from hops (Humulus lupulus). The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in negative ion electrospray mode. Reversed phase separation was carried out using a Waters XBridge 2.0 x 50mm C18 column (2.5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 20-95%B operating at a flow rate of 0.22 mL/min over 10 minutes was applied. Under these conditions the compound eluted at the retention time of 5.6 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 369 and a collision energy of 20eV.
Challenge 29
This molecule is a natural product isolated from a terrestrial plant. The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in positive ion electrospray mode. Reversed phase separation was carried out using a Hypersil GOLD 2.0 x 150mm C18 column (5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 6-50%B operating at a flow rate of 0.20mL/min over 30 minutes was applied. Under these conditions the compound eluted at the retention time of 17.8 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 338 and a collision energy of 25eV.
Challenge 30
This compound is a natural product isolated from several plants. The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in positive ion electrospray mode. Reversed phase separation was carried out using a Waters XBridge 2.0 x 50mm C18 column (2.5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 20-95%B operating at a flow rate of 0.22 mL/min over 10 minutes was applied. Under these conditions the compound eluted at the retention time of 8.5 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 473 and a collision energy of 15eV.
Challenge 31
This compound is a common natural product occurring in many plants, particularly in flowers and fruits. The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in positive ion electrospray mode. Reversed phase separation was carried out using a Waters XBridge 2.0 x 50mm C18 column (2.5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 25-80%B operating at a flow rate of 0.20 mL/min over 10 minutes was applied. Under these conditions the compound eluted at the retention time of 1.1 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 301 and a collision energy of 25eV.
Challenge 32
This molecule was detected in human serum with a retention time of 6347 seconds. The data were acquired applying UPLC-MS on a Thermo Scientific Ultimate3000 integrated with a Thermo Scientific Q Exactive mass spectrometer operating in electrospray positive ion mode. A Thermo Scientific GOLD C18 (2.1 mm × 100 mm, 1.9µm) column was applied. A reversed phase linear gradient elution operating at a flow rate of 0.35mL/min over 10 minutes from 5%A to 95%A was applied with water (+0.1% formic acid) as solvent A and methanol (+0.1% formic acid) as solvent B. The expected mass accuracy of the instrument is <5ppm. MS/MS data were acquired in positive ion mode applying HCD and m/z measurements in the Q Exactive with a precursor selection width of +/-1.5Da, a precursor m/z of 207 and a normalised collision energy of 40%. The expected mass accuracy for MS/MS data is <5ppm.
Challenge 33
The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in positive ion electrospray mode. Reversed phase separation was carried out using a Waters XBridge 2.0 x 50mm C18 column (2.5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 20-95%B operating at a flow rate of 0.22mL/min over 10 minutes was applied. Under these conditions the compound eluted at the retention time of 8.1 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 382 and a collision energy of 30eV.
Challenge 34
The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in positive ion electrospray mode. Reversed phase separation was carried out using a Waters XBridge 2.0 x 50mm C18 column (2.5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 20-95%B operating at a flow rate of 0.22mL/min over 10 minutes was applied. Under these conditions the compound eluted at the retention time of 4.5 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 394 and a collision energy of 30eV.
Challenge 35
This compound has long been considered a synthetic molecule and has been used for preparation of polymers as well as in the fragrance industry. Recently, the molecule has been identified as a natural product as well. The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in negative ion electrospray mode. Reversed phase separation was carried out using a Waters XBridge 2.0 x 50mm C18 column (2.5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 10-60%B operating at a flow rate of 0.22mL/min over 10 minutes was applied. Under these conditions the compound eluted at the retention time of 2.0 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 209 and a collision energy of 15eV.
Challenge 36
The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in positive ion electrospray mode. Reversed phase separation was carried out using a Waters XBridge 2.0 x 50mm C18 column (2.5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 20-95%B operating at a flow rate of 0.22mL/min over 10 minutes was applied. Under these conditions the compound eluted at the retention time of 2.1 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 210 and a collision energy of 15eV.
Challenge 37
The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in positive ion electrospray mode. Reversed phase separation was carried out using a Waters XBridge 2.0 x 50mm C18 column (2.5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 20-95%B operating at a flow rate of 0.22mL/min over 10 minutes was applied. Under these conditions the compound eluted at the retention time of 3.9 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 305 and a collision energy of 15eV.
Challenge 38
The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in positive ion electrospray mode. Reversed phase separation was carried out using a Waters XBridge 2.0 x 50mm C18 column (2.5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 20-95%B operating at a flow rate of 0.22mL/min over 10 minutes was applied. Under these conditions the compound eluted at the retention time of 7.7 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 426 and a collision energy of 25eV.
Challenge 39
The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in positive ion electrospray mode. Reversed phase separation was carried out using a Waters XBridge 2.0 x 50mm C18 column (2.5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 20-95%B operating at a flow rate of 0.22mL/min over 10 minutes was applied. Under these conditions the compound eluted at the retention time of 6.3 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 357 and a collision energy of 25eV.
Challenge 40
The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in negative ion electrospray mode. Reversed phase separation was carried out using a Waters XBridge 2.0 x 50mm C18 column (2.5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 20-95%B operating at a flow rate of 0.22mL/min over 10 minutes was applied. Under these conditions the compound eluted at the retention time of 6.0 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 227 and a collision energy of 25eV.
Challenge 41
The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in positive ion electrospray mode. Reversed phase separation was carried out using a Waters XBridge 2.0 x 50mm C18 column (2.5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 60-100%B operating at a flow rate of 0.20mL/min over 10 minutes was applied. Under these conditions the compound eluted as two peaks at the retention times of 4.0 and 4.2 min. Mass spectrometric data for both of these peaks were identical. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 523 and a collision energy of 25eV.
Challenge 42
The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in positive ion electrospray mode. Reversed phase separation was carried out using a Waters XBridge 2.0 x 50mm C18 column (2.5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 20-95%B operating at a flow rate of 0.22mL/min over 10 minutes was applied. Under these conditions the compound eluted at the retention time of 7.9 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 309 and a collision energy of 15eV.
Challenge 43
This molecule is an unreported natural product identified in a terrestrial plant. The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in positive ion electrospray mode. Reversed phase separation was carried out using a Hypersil GOLD 2.0 x 150mm C18 column (5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 6-65%B operating at a flow rate of 0.20mL/min over 30 minutes was applied. Under these conditions the compound eluted at the retention time of 8.6 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 381 and a collision energy of 20eV.
Challenge 44
This molecule is a synthetic derivative of a known natural product. The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in positive ion electrospray mode. Reversed phase separation was carried out using a Hypersil GOLD 2.0 x 150mm C18 column (5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 6-65%B operating at a flow rate of 0.20mL/min over 30 minutes was applied. Under these conditions the compound eluted at the retention time of 12.1 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 280 and a collision energy of 20eV.
Challenge 45
This molecule is an unreported natural product identified in a terrestrial plant. The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in positive ion electrospray mode. Reversed phase separation was carried out using a Hypersil GOLD 2.0 x 150mm C18 column (5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 6-36%B operating at a flow rate of 0.20mL/min over 30 minutes was applied. Under these conditions the compound eluted at the retention time of 11.1 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 214 and a collision energy of 20eV.
Challenge 46
This molecule is an unreported natural product identified in a terrestrial plant. The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in positive ion electrospray mode. Reversed phase separation was carried out using a Hypersil GOLD 2.0 x 150mm C18 column (5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 6-36%B operating at a flow rate of 0.20mL/min over 30 minutes was applied. Under these conditions the compound eluted at the retention time of 10.8 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 323 and a collision energy of 15eV.
Challenge 47
This molecule can be considered an adduct of two primary metabolites occurring in living organisms. The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in positive ion electrospray mode. Reversed phase separation was carried out using a Hypersil GOLD 2.0 x 150mm C18 column (5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 30-90%B operating at a flow rate of 0.20mL/min over 30 minutes was applied. Under these conditions the compound eluted at the retention time of 20.8 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 451 and a collision energy of 25eV.
Challenge 48
This molecule is a synthetic derivative of a natural product. The contest data were acquired on a Waters 2695 solvent delivery system integrated with a Waters SYNAPT quadrupole/time-of flight (QTOF) mass spectrometer operating in positive ion electrospray mode. Reversed phase separation was carried out using a Hypersil GOLD 2.0 x 150mm C18 column (5 µm particle size) and a mobile phase consisting of water + 0.1% formic acid as solvent A and acetonitrile as solvent B. A linear gradient from 6-65%B operating at a flow rate of 0.20mL/min over 30 minutes was applied. Under these conditions the compound eluted at the retention time of 6.0 min. The expected mass accuracy of the instrument is <5ppm in MS mode or < 10ppm (or < 1.8mDa) in MS/MS mode. MS/MS data were acquired using CID with argon as a collision gas, with a precursor selection width of +/ 1.5 Da, a precursor m/z of 280 and a collision energy of 25eV.