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A comparison of sorptive extraction techniques coupled to a new quantitative, sensitive, high throughput GC-MS/MS method for methoxypyrazine analysis in wine.
Talanta. 2016 Feb 01; 148:336-45.T

Abstract

Methoxypyrazines are volatile compounds found in plants, microbes, and insects that have potent vegetal and earthy aromas. With sensory detection thresholds in the low ng L(-1) range, modest concentrations of these compounds can profoundly impact the aroma quality of foods and beverages, and high levels can lead to consumer rejection. The wine industry routinely analyzes the most prevalent methoxypyrazine, 2-isobutyl-3-methoxypyrazine (IBMP), to aid in harvest decisions, since concentrations decrease during berry ripening. In addition to IBMP, three other methoxypyrazines IPMP (2-isopropyl-3-methoxypyrazine), SBMP (2-sec-butyl-3-methoxypyrazine), and EMP (2-ethyl-3-methoxypyrazine) have been identified in grapes and/or wine and can impact aroma quality. Despite their routine analysis in the wine industry (mostly IBMP), accurate methoxypyrazine quantitation is hindered by two major challenges: sensitivity and resolution. With extremely low sensory detection thresholds (~8-15 ng L(-1) in wine for IBMP), highly sensitive analytical methods to quantify methoxypyrazines at trace levels are necessary. Here we were able to achieve resolution of IBMP as well as IPMP, EMP, and SBMP from co-eluting compounds using one-dimensional chromatography coupled to positive chemical ionization tandem mass spectrometry. Three extraction techniques HS-SPME (headspace-solid phase microextraction), SBSE (stirbar sorptive extraction), and HSSE (headspace sorptive extraction) were validated and compared. A 30 min extraction time was used for HS-SPME and SBSE extraction techniques, while 120 min was necessary to achieve sufficient sensitivity for HSSE extractions. All extraction methods have limits of quantitation (LOQ) at or below 1 ng L(-1) for all four methoxypyrazines analyzed, i.e., LOQ's at or below reported sensory detection limits in wine. The method is high throughput, with resolution of all compounds possible with a relatively rapid 27 min GC oven program.

Authors+Show Affiliations

Department of Viticulture and Enology, University of California, Davis, Davis, CA 95616, USA; Food Safety and Measurement Facility, University of California, Davis, Davis, CA 95616, USA.Agilent Technologies, Inc., Wilmington, DE 19808, USA.Department of Viticulture and Enology, University of California, Davis, Davis, CA 95616, USA; Food Safety and Measurement Facility, University of California, Davis, Davis, CA 95616, USA. Electronic address: seebeler@ucdavis.edu.

Pub Type(s)

Comparative Study
Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

26653458

Citation

Hjelmeland, Anna K., et al. "A Comparison of Sorptive Extraction Techniques Coupled to a New Quantitative, Sensitive, High Throughput GC-MS/MS Method for Methoxypyrazine Analysis in Wine." Talanta, vol. 148, 2016, pp. 336-45.
Hjelmeland AK, Wylie PL, Ebeler SE. A comparison of sorptive extraction techniques coupled to a new quantitative, sensitive, high throughput GC-MS/MS method for methoxypyrazine analysis in wine. Talanta. 2016;148:336-45.
Hjelmeland, A. K., Wylie, P. L., & Ebeler, S. E. (2016). A comparison of sorptive extraction techniques coupled to a new quantitative, sensitive, high throughput GC-MS/MS method for methoxypyrazine analysis in wine. Talanta, 148, 336-45. https://doi.org/10.1016/j.talanta.2015.10.086
Hjelmeland AK, Wylie PL, Ebeler SE. A Comparison of Sorptive Extraction Techniques Coupled to a New Quantitative, Sensitive, High Throughput GC-MS/MS Method for Methoxypyrazine Analysis in Wine. Talanta. 2016 Feb 1;148:336-45. PubMed PMID: 26653458.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - A comparison of sorptive extraction techniques coupled to a new quantitative, sensitive, high throughput GC-MS/MS method for methoxypyrazine analysis in wine. AU - Hjelmeland,Anna K, AU - Wylie,Philip L, AU - Ebeler,Susan E, Y1 - 2015/10/30/ PY - 2015/07/20/received PY - 2015/10/28/revised PY - 2015/10/29/accepted PY - 2015/12/15/entrez PY - 2015/12/15/pubmed PY - 2016/9/22/medline KW - Aroma KW - Grape KW - HS-SPME KW - HSSE KW - IBMP KW - IPMP KW - Methoxypyrazines KW - SBSE KW - Wine SP - 336 EP - 45 JF - Talanta JO - Talanta VL - 148 N2 - Methoxypyrazines are volatile compounds found in plants, microbes, and insects that have potent vegetal and earthy aromas. With sensory detection thresholds in the low ng L(-1) range, modest concentrations of these compounds can profoundly impact the aroma quality of foods and beverages, and high levels can lead to consumer rejection. The wine industry routinely analyzes the most prevalent methoxypyrazine, 2-isobutyl-3-methoxypyrazine (IBMP), to aid in harvest decisions, since concentrations decrease during berry ripening. In addition to IBMP, three other methoxypyrazines IPMP (2-isopropyl-3-methoxypyrazine), SBMP (2-sec-butyl-3-methoxypyrazine), and EMP (2-ethyl-3-methoxypyrazine) have been identified in grapes and/or wine and can impact aroma quality. Despite their routine analysis in the wine industry (mostly IBMP), accurate methoxypyrazine quantitation is hindered by two major challenges: sensitivity and resolution. With extremely low sensory detection thresholds (~8-15 ng L(-1) in wine for IBMP), highly sensitive analytical methods to quantify methoxypyrazines at trace levels are necessary. Here we were able to achieve resolution of IBMP as well as IPMP, EMP, and SBMP from co-eluting compounds using one-dimensional chromatography coupled to positive chemical ionization tandem mass spectrometry. Three extraction techniques HS-SPME (headspace-solid phase microextraction), SBSE (stirbar sorptive extraction), and HSSE (headspace sorptive extraction) were validated and compared. A 30 min extraction time was used for HS-SPME and SBSE extraction techniques, while 120 min was necessary to achieve sufficient sensitivity for HSSE extractions. All extraction methods have limits of quantitation (LOQ) at or below 1 ng L(-1) for all four methoxypyrazines analyzed, i.e., LOQ's at or below reported sensory detection limits in wine. The method is high throughput, with resolution of all compounds possible with a relatively rapid 27 min GC oven program. SN - 1873-3573 UR - https://www.unboundmedicine.com/medline/citation/26653458/A_comparison_of_sorptive_extraction_techniques_coupled_to_a_new_quantitative_sensitive_high_throughput_GC_MS/MS_method_for_methoxypyrazine_analysis_in_wine_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0039-9140(15)30452-5 DB - PRIME DP - Unbound Medicine ER -