Present study describes the optimization of disk type sorptive extraction using monolithic material (Mono Trap) for the analysis of volatile aroma compounds from Lantana camara L. in combination with gas chromatography/mass spectrometry (GC/MS). Monolithic material sorptive extraction (MMSE) is a new sampling technique using a monolithic hybrid adsorptive disk (O.D. 10 mm, 1 mm thickness) made of high purity silica and activated carbon having a large surface area chemically bonded with octadecyl silane (ODS). The experimental parameters that may influence the MMSE efficiency have been optimized. Linearity, accuracy, precision and detection limits were evaluated to assess the performance of the proposed method. The method was validated with real plant samples of Lantana camara L. Twenty eight compounds including the main representative compounds of α-curcumene and β-caryophyllene were found in analyzed samples. Results proved that proposed method could be used as a good alternative for the analysis for such volatile aroma compounds in plant samples.
A prototype stainless steel needle (Hamilton 90022, 22 gauge, 718 µm o.d., 413 µm i.d., 51 mm length, bevel tip) packed with polyacrylic acid (PAA) and polydimethylsiloxane (PDMS) mixture (7:3 ratio) having a micro‐bore tunnel (290 µm i.d., ca. 61.5 µm thickness, 10 mm length) was newly prepared as a device of headspace in‐needle microextraction (HS‐INME). Design of the needle, optimization of adsorption, desorption parameters, and validation of analytical methods were conducted to evaluate the HS‐INME efficiency for volatile organic compounds. The optimized adsorption conditions were 60 °C for 20 min and desorption conditions were 240 °C for 2 min. The calibration curves showed good linearity with the squared correlation coefficient value (r2) over 0.99. The limit of detection for linalool, (+)‐limonene, and eugenol were 13.5, 10.9, and 9.1 ng while limit of quantification were 45.1, 36.4, and 30.5 ng, respectively. The recovery results showed the acceptable range between 95.6 and 115.3%. The relative standard deviations for intra‐ and inter‐assay showed the values less than 10%. It was applied to analyze seven essential oils for polar and nonpolar volatile aroma compounds successfully. From the results obtained in this study, HS‐INME was advantageous to low cost due to ease of fabrication, reuse without loss of absorbent or reduction of extraction efficiency, and no use of solvent. In conclusion, a needle packed with PAA and PDMS mixture having a micro‐bore tunnel is a new development of INME that may complement the shortcomings of the current headspace extraction methods.
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