Quantitative Analysis of Terpenic Compounds in Microsamples of Resins by Capillary Liquid Chromatography

Abstract

A method has been developed for the separation and quantification of terpenic compounds typically used as markers in the chemical characterization of resins based on capillary liquid chromatography coupled to UV detection. The sample treatment, separation and detection conditions have been optimized in order to analyze compounds of different polarities and volatilities in a single chromatographic run. The monoterpene limonene and the triterpenes lupeol, lupenone, β-amyrin, and α-amyrin have been selected as model compounds. The proposed method provides linear responses and precision (expressed as relative standard deviations) of 0.6% to 17%, within the 0.5–10.0 µg mL−1 concentration interval; the limits of detection (LODs) and quantification (LOQs) were 0.1–0.25 µg mL−1 and 0.4–0.8 µg mL−1, respectively. The method has been applied to the quantification of the target compounds in microsamples. The reliability of the proposed conditions has been tested by analyzing three resins, white copal, copal in tears, and ocote tree resin. Percentages of the triterpenes in the range 0.010% to 0.16% were measured using sample amounts of 10–15 mg, whereas the most abundant compound limonene (≥0.93%) could be determined using 1 mg portions of the resins. The proposed method can be considered complementary to existing protocols aimed at establishing the chemical fingerprint of these kinds of samples.

Determination of Limonene Chirality in Oils Obtained from Different Types of Citrus Waste Peels in Türkiye

“…The LODs of Rlimonene and S-limonene were found to be 0.08 mg/L and 0.09 mg/L, while their LOQs were calculated as 0.24 mg/L and 0.26 mg/L, respectively. As seen in Table 2, the values of LODs and LOQs of both limonenes are at a level comparable to studies in the literature in this field (31)(32)(33). The accuracy test involved injecting a standard solution with a concentration of 5 mg/L into the mixture of citrus oils and taking six measurements to calculate the recovery of each limonene.…”

Hand-Portable Miniaturized Liquid Chromatography for the Determination of Chlorogenic Acids in Dietary Supplements

“…Miniaturized separation techniques have proved to be very useful in the identification and determination of several classes of compounds present in complex samples. Compared with conventional scale LC, miniaturized LC, such as capLC and nanoLC, provides enhanced resolution and detection capabilities; thus, it is increasingly used in many fields of application [ 18 , 19 , 20 ], including samples of a botanical origin [ 21 ]. However, in the analysis of dietary supplements, miniaturized LC has only been applied to a few amino acids, peptides, fatty acids, and flavonoids [ 22 ].…”

The Effect of Ferula communis Extract in Escherichia coli Lipopolysaccharide-Induced Neuroinflammation in Cultured Neurons and Oligodendrocytes

“…These compounds can be extracted from a wide range of plants, and their basic chemical structure consists of a number of repeated isoprene (C 5 H 8 ) units [ 3 , 4 ]. The main terpenic compounds are monoterpenes (C10), sesquiterpenes (C15), diterpenes (C20), triterpenes (C30), and tetraterpenes (C40) [ 5 ]. The most beneficial effects of terpenic compounds are their antioxidant properties [ 6 ], although their use as penetration enhancers for transdermal drug delivery has recently become widespread [ 7 ].…”