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Application News No. M288 Gas Chromatography New Approach to Food Smell Analysis Using Combination of GCMS™ and GC-SCD (1) Gas chromatography mass spectrometry (GCMS), which has outstanding qualitative analysis capabilities, is used in smell analyses of food products, but because sulfur compounds contribute to the smell of food, even when present in trace amounts, detection by GCMS is difficult in some cases due to insufficient sensitivity and separation of sulfur compounds from other components. In this experiment, we studied a new approach to analysis of food smell by using a combination of GCMS, which is particularly effective for comprehensive qualitative analysis of odor components, and a GC device equipped with a sulfur chemiluminescence detector (GC- SCD), which enables selective and highly sensitive detection of only sulfur compounds. As the study method, an analysis of the smell released into the outside air from a storage bag was conducted using kimchi (Korean pickles) which has a particular strong smell among food products as the sample. Y. Takemori, K. Kawamura, T. Ishii Appearance of GCMS-QP™2020 NX + Nexis™ SCD-2030 Sample and Analysis Method Using commercially-available kimchi as the sample material, a sample was prepared by the following procedure. (1) Place 5 g of kimchi in a bag (polyethylene) and seal. (2) Place the sample prepared in (1) and 4 pieces of MonoTrap (DCC-18, GL Sciences Inc.) in a wide-mouth vial and seal. (3) Allow to stand for 2 h at room temperature. (4) Remove the MonoTrap from the wide-mouth vial. (5) Conduct solvent extraction of the MonoTrap in (4) using 1 mL of a mixed liquid of diethyl ether and n-pentane (1: 1). Analysis Conditions Table 1 shows the composition of the GC instrument and the analysis conditions used in this experiment. Table 2 shows the composition of the GCMS instrument and the analysis conditions. Table 1 Composition of GC Instrument and Analysis Conditions Model : Nexis GC-2030/SCD-2030 Injection Volume : 1 μL Injection : SPL Injection Temp. : 250 °C Injection Mode : Split Split Ratio : 1:5 Carrier Gas : He Carrier Gas Control : Constant pressure (44.5 kPa) Column : InertCap 5MS/Sil (30 m×0.32 mm I.D., 0.50 μm) Column Temp. : 50 °C (5 min) – 10 °C /min – 250 °C (10 min) Detector : Sulfur chemiluminescence detector (SCD) Interface Temp. : 200 °C Electric Furnace Temp. : 850 °C Detector Gas : H2 80.0 mL/min N2 40.0 mL/min O2 10.0 mL/min O3 25.0 mL/min Table 2 Composition of GCMS Instrument and Analysis Conditions Model : GCMS-QP2020NX GC Injection Volume : 1 μL Injection : SPL Injection Temp. : 250 °C Injection Mode : Split Split Ratio : 1:5 Carrier Gas : He Carrier Gas Control : Constant pressure (44.5 kPa) Column : InertCap 5MS/Sil (30 m×0.32 mm I.D., 0.50 μm) Column Temp. : 50 °C (5 min) – 10 °C /min – 250 °C (10 min) MS (El method) Ion Source Temp. : 200 °C Interface Temp. : 250 °C Ionization Mode : EI Measurement Mode : Scan Event Time : 0.3 s Kimchi (5 g) Sealed bag MonoTrap Solvent extraction Sample Wide-mouth vial MonoTrap
First Edition: Feb. 2020 For Research Use Only. Not for use in diagnostic procedures. This publication may contain references to products that are not available in your country. Please contact us to check the availability of these products in your country. The content of this publication shall not be reproduced, altered or sold for any commercial purpose without the written approval of Shimadzu. Shimadzu disclaims any proprietary interest in trademarks and trade names used in this publication other than its own. See http://www.shimadzu.com/about/trademarks/index.html for details. The information contained herein is provided to you "as is" without warranty of any kind including without limitation warranties as to its accuracy or completeness. Shimadzu does not assume any responsibility or liability for any damage, whether direct or indirect, relating to the use of this publication. This publication is based upon the information available to Shimadzu on or before the date of publication, and subject to change without notice. © Shimadzu Corporation, 2020 www.shimadzu.com/an/ Application News No. M288 Analysis Results Fig. 1 shows the GC-SCD chromatogram, and Fig. 2 shows the GCMS total ion chromatogram (TIC). Use of GC-SCD enabled selective and highly sensitive analysis of 8 species of sulfur compounds. The scan analysis by GCMS could detect four species of the sulfur compounds, as well as other compounds such as alcohols and ketones. Table 3 shows the sulfur compounds detected in this experiment. From these results, comprehensive detection of odor components was possible by GCMS, while trace amounts of sulfur compounds could be detected by GC-SCD. Fig. 1 GC-SCD Chromatogram Fig. 2 GCMS Total Ion Chromatogram Table 3 Sulfur Compounds Detected in Experiment ID Compound Name ID Compound Name 1 Allyl Methyl Sulfide 5 Dimethyl trisulfide 2 S-methyltioacetate 6 4-Isothiocyanato-1-butene 3 Dimethyl disulfide 7 Diallyl disulfide 4 Allyl Methyl Disulfide 8 Trisulfide, methyl 2-propeny Conclusion An analysis of the odor leaked into the outside air from a bag in which kimchi was stored was carried out using a GC-SCD and GCMS. Eight species of sulfur compounds could be detected. The combination of GC-SCD and GCMS enabled easy identification of sulfur compounds, and also made it possible to detect sulfur components present only in trace amounts. GCMS, GCMS-QP, and Nexis are trademarks of Shimadzu Corporation in Japan and/or other countries. Third-party trademarks and trade names may be used in this publication to refer to either the entities or their products/services, whether or not they are used with trademark symbol “TM” or “£”. 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0 11.0 12.0 13.0 14.0 min 1 2 3 4 5 6 7 8 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0 11.0 12.0 13.0 14.0 15.0 3 4 5 6
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