A Comparison of Headspace Solid‐phase Microextraction and Classic Hydrodistillation for the Identification of Volatile Constituents from <i>Thapsia</i> spp. Provides Insights into Guaianolide Biosynthesis in Apiaceae

Drew, Damian Paul; Rasmussen, Søren K.; Avato, Pinarosa; Simonsen, Henrik Toft

doi:10.1002/pca.1323

Cited by 42 publications

(46 citation statements)

References 22 publications

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“…Sesquiterpene hydrocarbons and sesquiterpenoids with a single hydroxyl group are often very volatile, and these are best analyzed using gas chromatography (GC) combined with mass spectroscopy (MS) [2,3]. The first step of sesquiterpenoid biosynthesis is performed by sesquiterpene synthases (sqTPS) [4].…”

Section: Introductionmentioning

confidence: 99%

Optimization of Biochemical Screening Methods for Volatile and Unstable Sesquiterpenoids Using HS-SPME-GC-MS

2015

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HS-SPME-GC-MS has been suggested as a fast and robust analytical platform for the product characterization of sesquiterpene synthases. The choice of fiber and injection temperature can have a significant effect on the observed product profile, due to the chemical rearrangements that can occur on the fiber material. Here we present a systematic study on the effects of fiber choice and injection port temperature on the observed sesquiterpenoid profile of four sesquiterpene synthases expressed in Nicotiana benthamiana. We found that the absorbent material PDMS was much less likely to support acid-induced rearrangement of sesquiterpenoids when compared to the adsorbent materials PDMS/DVB, PDMS/CAR, and PDMS/CAR/DVB. Furthermore, utilizing an injection port temperature at 160 °C almost eliminated the inherent thermal instability of germacrene sesquiterpenoids. Thus, for fast screening of sesquiterpene synthases, the results suggest that PDMS fibers and an injection temperature of 160 °C provide a fast and reproducible HS-SPME GC-MS method when using H2 as carrier gas.

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Section: Introductionmentioning

confidence: 99%

Optimization of Biochemical Screening Methods for Volatile and Unstable Sesquiterpenoids Using HS-SPME-GC-MS

2015

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“…To evaluate the capability of this HS-SPME-GCMS method for distinguishing aflatoxigenic and non-aflatoxigenic A. flavus, the GCMS data (day 1,3,6,10,20,24,30) from fungi and control samples were collected and analyzed using discriminant analysis (DA) models. DA builds up a predictive model which is composed of a discriminant function based on linear combinations of predictor variables.…”

Section: Multivariate Analysis Of Mvoc Profilementioning

confidence: 99%

“…This technique has the potential to be part of an efficient method for field applications due to its portability and simplicity. The application of SPME in conjunction with GC-MS has been successfully applied to the detection of indoor mold [22] [23], fungal species identification [24] [25], and the diagnosis of foodborne pathogen infection [26] [27].…”

Section: Introductionmentioning

confidence: 99%

Monitoring MVOC Profiles over Time from Isolates of Aspergillus flavus Using SPME GC-MS

Sun¹,

Wood-Jones²,

Wang³

et al. 2014

JACEN

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Fungi produce a variety of microbial volatile organic compounds (MVOCs) during primary and secondary metabolism. The fungus, Aspergillus flavus, is a human, animal and plant pathogen which produces aflatoxin, one of the most carcinogenic substances known. In this study, MVOCs were analyzed using solid phase microextraction (SPME) combined with GCMS from two genetically different A. flavus strains, an aflatoxigenic strain, NRRL 3357, and a non-aflatoxigenic strain, NRRL 21882. A PDMS/CAR SPME fiber was used over 30 days to observe variations in MVOCs over time. The relative percentage of individual chemicals in several chemical classes (alcohols, aldehydes, esters, furans, hydrocarbons, ketones, and organic acids) was shown to change considerably during the varied fungal growth stages. This changing chemical profile reduces the likelihood of finding a single chemical that can be used consistently as a biomarker for fungal strain identification. In our study, discriminant analysis techniques were successfully conducted using all identified and quantified MVOCs enabling discrimination of the two A. flavus strains over the entire 30-day period. This study underscores the potential of using SPME GCMS coupled with multivariate analysis for fungi strain identification.

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“…Comparison of the compounds identified in the essential oil and those extracted by HS-SPME (Tables 1 and 2) suggested that significant chemical modifications could occur during hydrodistillation. The same differences have been reported during the analysis of other plants using both methods, which in turn raised the question about the true nature of the volatile compounds of the analyzed herbs (Drew et al, 2012). Dawidowicz et al (2008) attributed the differences in the components of the essential oil of Thymus vulgaris obtained by hydrodistillation and those found by HS-SPME were due to the nature of the fiber.…”

Section: Discussionmentioning

confidence: 80%

“…Gas chromatographic coupled to mass spectrometry (GC-MS) is widely used for identifying characteristic volatile compounds present in herbal drugs and to construct representative chromatographic profiles useful for their quality control (Drew et al, 2012). In the present investigation, the volatile constituents of C. filaginoides were initially established through the analysis of the essential oil obtained by hydrodistillation as required in most pharmacopeias (European, United States and Mexican Pharmacopeias, among others).…”

Section: Volatile Chemical Composition Analysismentioning

confidence: 99%

Quality control tests for the crude drug ofConyza filaginoides

Ovalle-Magallanes

Rivero‐Cruz

Mata

2013

Pharmaceutical Biology

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Context: Conyza filaginoides (D.C.) Hieron (Asteraceae) is a medicinal Mexican plant highly prized in contemporary Mexico for the treatment of upset stomach and diabetes. Objective: This work was undertaken to develop a suitable high performance liquid chromatography (HPLC)-diode array detection (DAD) method for quantifying rutin (1), the main active principle from the aerial parts of C. filaginoides. Materials and methods: The method was performed using a LiChrospher 100 RP-18 column. The mobile phase was water (containing 0.1% phosphoric acid)-methanol-acetonitrile (80:5:15, v/v) at a flow rate of 1.2 mL min À1. Results: Limits of detection and quantification were 7.5 and 22.8 mg mL À1, respectively. The main recoveries measured at three concentrations were higher than 98%, with RSD 52%. Quantitative analysis of a few samples showed the presence of high concentrations of 1 (3.6 AE 0.2 g/100 g of dry plant material). The volatile components were extracted by hydrodistillation or head space solid-phase microextraction (HS-SPME), and thereafter analyzed by gas chromatography coupled to mass spectrometry (GC-MS). Forty-three chemical constituents representing 90% of the total content of the oil were identified. The major light volatile compounds obtained by HS-SPME revealed a high content of monoterpene hydrocarbons.Conclusions: A precise, reliable, and accurate analytical HPLC method to detect and quantify 1 in the crude drug and some preparations were developed and fully validated. The volatile components of the plant are described for the first time. The proposed method would be useful for quality control assurance of this important Mexican plant.

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A Comparison of Headspace Solid‐phase Microextraction and Classic Hydrodistillation for the Identification of Volatile Constituents from Thapsia spp. Provides Insights into Guaianolide Biosynthesis in Apiaceae

Abstract: The new data reported in this study demonstrates that SPME is a valuable tool for the identification of volatile sesquiterpenes when compared with analysis of essential oils, and we postulate that guaiene is the likely precursor of guaianolide sesquiterpenes from Thapsia.

Cited by 42 publications

References 22 publications

Optimization of Biochemical Screening Methods for Volatile and Unstable Sesquiterpenoids Using HS-SPME-GC-MS

Optimization of Biochemical Screening Methods for Volatile and Unstable Sesquiterpenoids Using HS-SPME-GC-MS

Monitoring MVOC Profiles over Time from Isolates of Aspergillus flavus Using SPME GC-MS

Quality control tests for the crude drug ofConyza filaginoides

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