Fast GC-MS;
Low thermal mass gas chromatography;
Resistively heated capillary chromatography;
High-throughput analysis;
FAST GC-MS;
OPEN PROBE;
COLUMN;
OPTIMIZATION;
TEMPERATURE;
IONIZATION;
SYSTEM;
D O I:
10.1016/j.chroma.2019.460691
中图分类号:
Q5 [生物化学];
学科分类号:
071010 ;
081704 ;
摘要:
Conventional gas chromatography - mass spectrometry (GC-MS) takes 20-40 min per sample, which is undesirably slow in any application if speed can be increased while still meeting analytical needs. In this study, we achieved reasonably good separations with full analysis cycle times of less than 1 min by combining for the first time low-pressure (LP) GC-MS with low thermal mass (LTM) resistive-heating for rapid temperature ramping and cooling of the capillary column. The analytical column is threaded into the LTM thin-walled metal tubing in an instrumental device known as "LTM Fast GC" that is mounted at the top of the gas chromatograph in a detector port. The column inlet and outlet are connected to the GC injector and MS transfer line as usual. For LPGC-MS, a 40 cm, 0.1 mm. i.d. uncoated flow restrictor capillary connected at the injector is coupled with a 2.6 m, 0.25 mm i.d., 0.25 gm film thickness analytical column leading to the MS. Thus, the inlet operates at normal GC pressures, but the analytical column is under vacuum, which increases the optimal helium carrier gas flow velocity thereby increasing speed of full range separations while maintaining acceptable quality of chromatography. This column configuration in LTM-LPGC-MS trades a 64-fold gain in speed of analysis vs. standard GC-MS for a 4-fold loss in chromatographic peak capacity, thereby converting analysis time from minutes into seconds in common applications. For example, jet fuel containing fatty acid methyl esters (akin to biofuel) was separated in 25 s with <1 min full analysis cycle time. An EPA Method 8270 mixture of 76 analytes was also analyzed in <1 min full cycle time by LTM-LPGC-MS. Other examples include very fast analysis of heroin in a street drug powder and elucidation of a new organic synthetic compound. In this report, we describe and discuss the several advantageous and practical features of LTM-LPGC-MS, as well as its trade-offs. (C) 2019 Elsevier B.V. All rights reserved.
机构:
ARS, USDA, Wyndmoor, PA 19038 USA
Univ La Laguna, Fac Quim, Dept Quim Analit Nutr & Bromatol, San Cristobal la Laguna 38206, Tenerife, SpainARS, USDA, Wyndmoor, PA 19038 USA
Angel Gonzalez-Curbelo, Miguel
Lehotay, Steven J.
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机构:
ARS, USDA, Wyndmoor, PA 19038 USAARS, USDA, Wyndmoor, PA 19038 USA
Lehotay, Steven J.
Hernandez-Borges, Javier
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机构:
Univ La Laguna, Fac Quim, Dept Quim Analit Nutr & Bromatol, San Cristobal la Laguna 38206, Tenerife, SpainARS, USDA, Wyndmoor, PA 19038 USA
Hernandez-Borges, Javier
Angel Rodriguez-Delgado, Miguel
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h-index: 0
机构:
Univ La Laguna, Fac Quim, Dept Quim Analit Nutr & Bromatol, San Cristobal la Laguna 38206, Tenerife, SpainARS, USDA, Wyndmoor, PA 19038 USA
机构:
USDA, Eastern Reg Res Ctr, Wyndmoor, PA USAUSDA, Eastern Reg Res Ctr, Wyndmoor, PA USA
Lehotay, Steven J.
de Zeeuw, Jaap
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机构:
Restek Corp, Bellefonte, PA 16823 USAUSDA, Eastern Reg Res Ctr, Wyndmoor, PA USA
de Zeeuw, Jaap
Sapozhnikova, Yelena
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机构:
USDA, Eastern Reg Res Ctr, Wyndmoor, PA USAUSDA, Eastern Reg Res Ctr, Wyndmoor, PA USA
Sapozhnikova, Yelena
Michlig, Nicolas
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机构:
USDA, Eastern Reg Res Ctr, Wyndmoor, PA USA
Univ Nacl Litoral, Programa Invest & Anal Residuos & Contaminantes Q, Fac Ingn Quim, Santa Fe, ArgentinaUSDA, Eastern Reg Res Ctr, Wyndmoor, PA USA
Michlig, Nicolas
Hepner, Jana Rousova
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机构:
Restek Corp, Bellefonte, PA 16823 USAUSDA, Eastern Reg Res Ctr, Wyndmoor, PA USA
Hepner, Jana Rousova
Konschnik, Joseph D.
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机构:
Restek Corp, Bellefonte, PA 16823 USAUSDA, Eastern Reg Res Ctr, Wyndmoor, PA USA