Optimization and validation of an HS-SPME/GC-MS method for determining volatile organic compounds in dry-cured ham
The formation of volatile organic compounds (VOCs) in dry-cured ham is a result of different biochemical and enzymatic processes. Moreover, accurately quantifying these VOCs is challenging since ham is a complex matrix, which contains compounds from various chemical families and a wide range of vola...
| Main Authors: | , , , |
|---|---|
| Format: | Article |
| Language: | English |
| Published: |
Frontiers Media S.A.
2024-02-01
|
| Series: | Frontiers in Nutrition |
| Subjects: | |
| Online Access: | https://www.frontiersin.org/articles/10.3389/fnut.2024.1342417/full |
| _version_ | 1827367446161391616 |
|---|---|
| author | Katja Babič Katja Babič Lidija Strojnik Andrija Ćirić Nives Ogrinc Nives Ogrinc |
| author_facet | Katja Babič Katja Babič Lidija Strojnik Andrija Ćirić Nives Ogrinc Nives Ogrinc |
| author_sort | Katja Babič |
| collection | DOAJ |
| description | The formation of volatile organic compounds (VOCs) in dry-cured ham is a result of different biochemical and enzymatic processes. Moreover, accurately quantifying these VOCs is challenging since ham is a complex matrix, which contains compounds from various chemical families and a wide range of volatilities of different molecular masses. In this study, we systematically optimized and validated an analytical method for quantifying VOCs in dry-cured ham using headspace solid phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS). Optimal SPME conditions were determined through both an experimental procedure (one-factor-at-a-time) and response surface methodology (RSM), revealing that a 60-min equilibration at 70°C, a 60-min extraction at the same temperature, and a 4-min desorption time at 250°C provided the most favorable results. To enhance quantitation, twelve multiple internal standards (ISTDs) were employed to address and improve the quantitation of the 12 VOCs. Method validation covered aspects of linearity, limits of detection (LOD: 0.03–1.13 mg kg−1), limits of quantitation (LOQ: 0.09–3.41 mg kg−1), and working ranges (0.01–19.1 mg kg−1). The practical application of this optimized method was demonstrated by analyzing dry-cured ham samples (n = 4), sourced from the Slovenian market. The initial statistical evaluation indicates that different types of dry-cured hams can be differentiated (with an 83.1% of accuracy) according to their aromatic profile. However, a larger sample size would be required to provide a more comprehensive assessment. |
| first_indexed | 2024-03-08T09:06:34Z |
| format | Article |
| id | doaj.art-94436f5e3659496fb43294610053383f |
| institution | Directory Open Access Journal |
| issn | 2296-861X |
| language | English |
| last_indexed | 2024-03-08T09:06:34Z |
| publishDate | 2024-02-01 |
| publisher | Frontiers Media S.A. |
| record_format | Article |
| series | Frontiers in Nutrition |
| spelling | doaj.art-94436f5e3659496fb43294610053383f2024-02-01T04:39:24ZengFrontiers Media S.A.Frontiers in Nutrition2296-861X2024-02-011110.3389/fnut.2024.13424171342417Optimization and validation of an HS-SPME/GC-MS method for determining volatile organic compounds in dry-cured hamKatja Babič0Katja Babič1Lidija Strojnik2Andrija Ćirić3Nives Ogrinc4Nives Ogrinc5Jožef Stefan International Postgraduate School, Ljubljana, SloveniaDepartment of Environmental Sciences, Jožef Stefan Institute, Ljubljana, SloveniaDepartment of Environmental Sciences, Jožef Stefan Institute, Ljubljana, SloveniaDepartment of Chemistry, Faculty of Science, University of Kragujevac, Kragujevac, SerbiaJožef Stefan International Postgraduate School, Ljubljana, SloveniaDepartment of Environmental Sciences, Jožef Stefan Institute, Ljubljana, SloveniaThe formation of volatile organic compounds (VOCs) in dry-cured ham is a result of different biochemical and enzymatic processes. Moreover, accurately quantifying these VOCs is challenging since ham is a complex matrix, which contains compounds from various chemical families and a wide range of volatilities of different molecular masses. In this study, we systematically optimized and validated an analytical method for quantifying VOCs in dry-cured ham using headspace solid phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS). Optimal SPME conditions were determined through both an experimental procedure (one-factor-at-a-time) and response surface methodology (RSM), revealing that a 60-min equilibration at 70°C, a 60-min extraction at the same temperature, and a 4-min desorption time at 250°C provided the most favorable results. To enhance quantitation, twelve multiple internal standards (ISTDs) were employed to address and improve the quantitation of the 12 VOCs. Method validation covered aspects of linearity, limits of detection (LOD: 0.03–1.13 mg kg−1), limits of quantitation (LOQ: 0.09–3.41 mg kg−1), and working ranges (0.01–19.1 mg kg−1). The practical application of this optimized method was demonstrated by analyzing dry-cured ham samples (n = 4), sourced from the Slovenian market. The initial statistical evaluation indicates that different types of dry-cured hams can be differentiated (with an 83.1% of accuracy) according to their aromatic profile. However, a larger sample size would be required to provide a more comprehensive assessment.https://www.frontiersin.org/articles/10.3389/fnut.2024.1342417/fulldry-cured hamHS-SPME/GC-MSoptimizationresponse surface methodologyvalidation |
| spellingShingle | Katja Babič Katja Babič Lidija Strojnik Andrija Ćirić Nives Ogrinc Nives Ogrinc Optimization and validation of an HS-SPME/GC-MS method for determining volatile organic compounds in dry-cured ham Frontiers in Nutrition dry-cured ham HS-SPME/GC-MS optimization response surface methodology validation |
| title | Optimization and validation of an HS-SPME/GC-MS method for determining volatile organic compounds in dry-cured ham |
| title_full | Optimization and validation of an HS-SPME/GC-MS method for determining volatile organic compounds in dry-cured ham |
| title_fullStr | Optimization and validation of an HS-SPME/GC-MS method for determining volatile organic compounds in dry-cured ham |
| title_full_unstemmed | Optimization and validation of an HS-SPME/GC-MS method for determining volatile organic compounds in dry-cured ham |
| title_short | Optimization and validation of an HS-SPME/GC-MS method for determining volatile organic compounds in dry-cured ham |
| title_sort | optimization and validation of an hs spme gc ms method for determining volatile organic compounds in dry cured ham |
| topic | dry-cured ham HS-SPME/GC-MS optimization response surface methodology validation |
| url | https://www.frontiersin.org/articles/10.3389/fnut.2024.1342417/full |
| work_keys_str_mv | AT katjababic optimizationandvalidationofanhsspmegcmsmethodfordeterminingvolatileorganiccompoundsindrycuredham AT katjababic optimizationandvalidationofanhsspmegcmsmethodfordeterminingvolatileorganiccompoundsindrycuredham AT lidijastrojnik optimizationandvalidationofanhsspmegcmsmethodfordeterminingvolatileorganiccompoundsindrycuredham AT andrijaciric optimizationandvalidationofanhsspmegcmsmethodfordeterminingvolatileorganiccompoundsindrycuredham AT nivesogrinc optimizationandvalidationofanhsspmegcmsmethodfordeterminingvolatileorganiccompoundsindrycuredham AT nivesogrinc optimizationandvalidationofanhsspmegcmsmethodfordeterminingvolatileorganiccompoundsindrycuredham |