HS-SPME-GC-MS Analyses of Volatiles in Plant Populations—Quantitating Compound × Individual Matrix Effects

Abstract

Headspace solid-phase microextraction (HS-SPME) coupled to gas chromatography–mass spectrometry (GC-MS) is widely employed for volatile analyses of plants, including mapping populations used in plant breeding research. Studies often employ a single internal surrogate standard, even when multiple analytes are measured, with the assumption that any relative changes in matrix effects among individuals would be similar for all compounds, i.e., matrix effects do not show Compound × Individual interactions. We tested this assumption using individuals from two plant populations: an interspecific grape (Vitis spp.) mapping population (n = 140) and a tomato (Solanum spp.) recombinant inbred line (RIL) population (n = 148). Individual plants from the two populations were spiked with a cocktail of internal standards (n = 6, 9, respectively) prior to HS-SPME-GC-MS. Variation in the relative responses of internal standards indicated that Compound × Individual interactions exist but were different between the two populations. For the grape population, relative responses among pairs of internal standards varied considerably among individuals, with a maximum of 249% relative standard deviation (RSD) for the pair of [U13C]hexanal and [U13C]hexanol. However, in the tomato population, relative responses of internal standard pairs varied much less, with pairwise RSDs ranging from 8% to 56%. The approach described in this paper could be used to evaluate the suitability of using surrogate standards for HS-SPME-GC-MS studies in other plant populations.

Berry Anthocyanin, Acid, and Volatile Trait Analyses in a Grapevine-Interspecific F2 Population Using an Integrated GBS and rhAmpSeq Genetic Map

“…Quantification of herbaceous volatiles (hexanal, (E)-2-hexenal, and 3-isopropyl-2-methoxypyrazine (IPMP), in 2013 and 2018 berry samples was carried out by headspace solid phase microextraction (HS-SPME; LEAP CombiPALAutosampler Carrboro, NC. USA) coupled to a Shimadzu gas chromatograph-mass spectrometer (GC-MS) (GC2010 Plus w/TQ8040 MS; Nakagyo-ku, Kyoto, Japan) by adapting a method described by Burzynski-Chang et al 2018 [ 70 ]. Frozen whole berries (25–50 g) were destemmed and macerated for one min using a chilled 250 mL stainless steel Waring blender.…”

A Rapid Gas-Chromatography/Mass-Spectrometry Technique for Determining Odour Activity Values of Volatile Compounds in Plant Proteins: Soy, and Allergen-Free Pea and Brown Rice Protein

“…Even though GC/MS has a high sensitivity for volatile detection, the matrix effect presented by individual proteins influences the accuracy of volatile compound quantification [ 22 ]. However, we observed that the calibration of soy and pea proteins could be changed interchangeably, which is probably attributed to both having a high concentration of proteins as the major compounds.…”

Broad diversity in monoterpene–sesquiterpene balance across wild sunflowers: Implications of leaf and floral volatiles for biotic interactions

“…Plant volatile profiles were determined by headspace solid‐phase microextraction gas chromatography‐mass spectrometry (SPME GC‐MS; Adam et al, 2005; Deng et al, 2006; Zhu et al, 2013; Burzynski‐Chang et al, 2018; Tholl et al, 2021) using a single quadrupole QP2020 (Shimadzu, Kyoto, Japan). For this purpose, leaf and petal samples were ground to homogeneity in liquid nitrogen, and ~50 mg of tissue was added to 10‐mL glass headspace vials with the total sample mass recorded.…”