Determination Of Terpenoids Research Articles

Extraction and determination of terpenoids from Zexie Decoction based on a porous organic cage-doped monolithic cartridge

A monolithic solid-phase extraction (SPE) cartridge packed with a composite adsorbent was fabricated via polymerization using dodecene as the monomer with the porous organic cage (POC) material doped, combing with an analytical column through a high-performance liquid chromatography (HPLC) instrument, which was used for the online extraction and separation of 23-acetyl alismol C, atractylodes lactone II and atractylodes lactone III from Zexie Decoction. The POC-doped adsorbent shows porous structure with a relatively high specific surface area of 85.50 m2/g, which was obtained from the characterizations of a scanning electron microscope and an automatic surface area and porosity analyser. Efficient extraction and separation of three target terpenoids was achieved by an online SPE-HPLC method based on the POC-doped cartridge, which exhibits strong matrix-removal ability and good terpenoids-retention ability with a high adsorption capacity, due to the interactions of hydrogen bond and hydrophobicity between the terpenoids and the POC-doped adsorbent. Method validation shows good linearity (r ≥ 0.9998) of the regression equation, and high accuracy with the spiked recovery in the range of 99.2 %-100.8 % of the proposed method. Compared to the generally disposable adsorbent, this work fabricated a reusable monolithic cartridge, which can be used for at least 100 times, with the RSD based on the peak area of the three terpenoids less than 6.6 %.

Determination of terpenoids in Baijiu using solid-phase extraction combined with headspace solid-phase microextraction

ABSTRACT A new method based on solid-phase extraction (SPE) combined with headspace solid-phase microextraction (HS-SPME) was established for the determination of terpenes in Baijiu. Terpenes were concentrated on the C18 solid-phase extraction column, and an additional enrichment of the terpenes was performed using HS-SPME for fillers of the C18 solid-phase extraction column. The conditions of the SPE and SPME were optimized, and the optimal conditions were using the Thermo C18 extraction column, elution water of 1 mL, an extraction temperature of 70°C, and an extraction time of 50 min. Under these optimal conditions, four terpenes were randomly selected to verify the analytical method in terms of linearity, the limit of detection, the limit of quantification, precision, and accuracy. The results showed that the SPE-HS-SPME method has high sensitivity and a high recovery rate, which was also accurate and reliable in the quantitative analysis. It is a feasible new method for the detection of terpene substances in Baijiu.

Determination of Terpenoids in Chamaecyparis obtusa Leaves by Headspace Single-Drop Microextraction with Gas Chromatography Detection

Headspace single-drop microextraction (HS-SDME) was used to extract five terpenoids (α-terpinene, γ-terpinene, linalool, α-terpineol, and terpinyl acetate) from powdered Chamaecyparis obtusa leaves. The terpenoids were determined by gas chromatography with flame ionization detection. Under the optimized conditions, oleyl alcohol efficiently extracted the analytes from the leaves within 20 min at 100°C. The results showed that the amounts of α-terpinene, γ-terpinene, linalool, α-terpineol, and terpinyl acetate extracted from the samples were 2.19, 3.68, 0.11, 0.87, and 22.35 µg/g, respectively. Compared to microextraction of the compounds from the sample solution, the new technique had fewer steps. The method also had similar extraction properties as heat reflux extraction, but required a smaller sample volume and less time.

Determination of Terpenoids in Plant Leaves by GC-MS: Development of the Method and Application to Ocimum basilicum and Nicotiana langsdorffii

In this work a simple and sensitive analytical method was developed for the determination of terpenoids in plants using gas chromatography coupled to mass spectrometry (GC-MS). Three extraction methods were tested on Ocimum basilicum leaves to maximize terpene extraction: Steam Distillation, Ultrasound-Assisted Extraction, and Microwave-Assisted Extraction (MAE). Best results, both in number of identified compounds and in their concentration, were obtained with MAE, which was used in all subsequent analyses. In particular five terpenoids (α-pinene, β-pinene, limonene, linalool, and α-terpineol) were chosen for the quantitative determination, performed in Selected Ion Monitoring mode. Calibration curves using dodecane as internal standard were drawn, showing good correlation coefficients (0.9981–0.9993). All figures of merit were satisfactory; limits of detection were in the range 14–27 ng for all analytes. The method was also applied to some specimens of wild-type and transgenic (GR and rolC) Nicotiana langsdorffii. Plants were exposed to water and chemical stresses to evaluate possible effects on terpene content. Linalool was present in higher quantities in the plants GR and rolC; both stresses produce a decrease of its concentration if compared to the non-stressed plants. The concentration of α-terpineol, detected only in WT and GR plants, was higher for the genetically modified plant, substantially confirming the trend observed for linalool.

Rapid simultaneous quantitative determination of terpenoids in Tripterygium wilfordii Hook F by ultra-high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry

A rapid and sensitive method for simultaneous quantitative determination of terpenoids in Tripterygium wilfordii Hook F (TwHF) was developed by ultra-high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UHPLC-QTOF-MS). In this method, five major terpenoids, including triptolide, triptonide, demethylzelastral, tripterine and wilforlide A, with large content range in TwHF, were determined simultaneously in a UHPLC run of 4.5 minutes. The intra-day and inter-day precisions of five terpenoids were less than 4.58% and 4.82%, respectively, and the mean recovery rates obtained were in the range of 97.2% to 104.5%. All calibration curves showed good linearity (r2 > 0.996) from 20 ng mL−1 and 20 000 ng mL−1. The limit of detection (LOD) and limit of quantitation (LOQ) were less than 5.7 ng mL−1 and 19.0 ng mL−1. Compared with previous studies, this method could be employed for accurate quantification of five terpenoids in different parts and products of TwHF in a very short time after simple ultrasonic extraction. The results indicated that this method would provide a rapid and sensitive way for evaluating the quality of the TwHF and its products.

Determination of terpenoids in wines by solid phase extraction and gas chromatography

A new method for determination of volatile terpenoids in wine is proposed. An off-line solid phase extraction—gas chromatographic method has been used for the determination. The influence of several extraction variables was studied, including the solid phase employed (C-18 versus divinylbenzene-based), eluting solvent ( n -pentane, dichloromethane, ethanol and methanol), volume of eluting solvent (1–4 ml) and drying time (0–20 min). Complete recovery of volatile terpenoids from several kinds of wines was obtained under the optimized conditions.

Determination of terpenoids in wines by solid phase extraction and gas chromatography

A new method for determination of volatile terpenoids in wine is proposed. An off-line solid phase extraction—gas chromatographic method has been used for the determination. The influence of several extraction variables was studied, including the solid phase employed (C-18 versus divinylbenzene-based), eluting solvent ( n-pentane, dichloromethane, ethanol and methanol), volume of eluting solvent (1–4 ml) and drying time (0–20 min). Complete recovery of volatile terpenoids from several kinds of wines was obtained under the optimized conditions.