Ionic liquid vortex‐simplified matrix solid‐phase dispersion for the simultaneous determination of terpenoids,crocins, quinic acid derivatives and flavonoids in Gardeniae fructus by UHPLC

A novel ionic‐liquid‐based vortex‐simplified matrix solid‐phase dispersion method using 2,6‐dimethyl‐β‐cyclodextrin was established by ultra high performance liquid chromatography coupled with a photodiode array detector. 2,6‐Dimethyl‐β‐cyclodextrin was first used as a promising adsorbent in this proposed method for simultaneous determination of eight compounds in Gardeniae fructus. These compounds are terpenoids (geniposidic acid, genipin‐1‐β‐D‐gentiobioside, geniposide, 8‐o‐acetyl shanzhiside methyl ester), crocins (crocin‐I, crocin‐II), quinic acid derivatives (chlorogenic acid), and flavonoids (isoquercitrin), respectively. Several parameters were investigated in the adsorption and desorption processes to obtain the optimal conditions, including 2,6‐dimethyl‐β‐cyclodextrin as sorbent, 0.5 mL 100 mM 1‐dodecyl‐3‐methylimidazolium hydrogen sulfate as the extraction solvent, 2:1 of sample/sorbent ratio, grinding for 2 min and vortexing for 60 s. The recoveries of the eight compounds ranged from 96.6 to 100% (<3.50%). The limits of detection and quantification were in the range of 0.02–0.30 and 0.06–1.25  μg/mL, respectively. Meanwhile, a good linearity was attained with r values (>0.9997). The established method showed higher extraction efficiency and less reagent consumption than traditional matrix solid phase dispersion and ultrasonic‐assisted extraction. Hence, it could be applied for sample preparation and analysis of natural products.     

A rapid and efficient extraction method based on industrial MCM‐41‐miniaturized matrix solid‐phase dispersion extraction with response surface methodology for simultaneous quantification of six flavonoids in Pollen typhae by ultra‐high‐performance liquid chromatography

An industrial MCM‐41‐miniaturized matrix solid‐phase dispersion extraction coupled with response surface methodology was explored to determine L‐epicatechin, typhaneoside, isorhamnetin‐3‐O‐neohespeidoside, naringenin, kaempferol, and isorhamnetin in Pollen typhae by ultra‐high performance liquid chromatography connected to a photodiode array detection. Several variables were optimized in detail, including mesh number of sieve, type of adsorbent, mass ratio of sample to adsorbent, grinding time, methanol concentration, and elution volume. Central composite design was applied to optimize the best conditions for the maximum yields of the total flavonoids. The results displayed a good linear relationship (R > 0.9992) and the recoveries ranged from 92.9 to 103% (RSD < 4.53%) of the six flavonoids. The optimal method with high efficiency and low consumption was obviously better than heating reflux and ultrasonic extraction. It was proven that the developed industrial MCM‐41‐miniaturized matrix solid‐phase dispersion extraction coupled with simple ultra‐high performance liquid chromatography method could be a rapid and efficient tool for extraction and determination of flavonoids in natural products.     

Design of guanidinium ionic liquid based microwave‐assisted extraction for the efficient extraction of Praeruptorin A from Radix peucedani

A series of novel tetramethylguanidinium ionic liquids and hexaalkylguanidinium ionic liquids have been synthesized based on 1,1,3,3‐tetramethylguanidine. The structures of the ionic liquids were confirmed by ¹H NMR spectroscopy and mass spectrometry. A green guanidinium ionic liquid based microwave‐assisted extraction method has been developed with these guanidinium ionic liquids for the effective extraction of Praeruptorin A from Radix peucedani. After extraction, reversed‐phase high‐performance liquid chromatography with UV detection was employed for the analysis of Praeruptorin A. Several significant operating parameters were systematically optimized by single‐factor and L₉ (3⁴) orthogonal array experiments. The amount of Praeruptorin A extracted by [1,1,3,3‐tetramethylguanidine]CH₂CH(OH)COOH is the highest, reaching 11.05 ± 0.13 mg/g. Guanidinium ionic liquid based microwave‐assisted extraction presents unique advantages in Praeruptorin A extraction compared with guanidinium ionic liquid based maceration extraction, guanidinium ionic liquid based heat reflux extraction and guanidinium ionic liquid based ultrasound‐assisted extraction. The precision, stability, and repeatability of the process were investigated. The mechanisms of guanidinium ionic liquid based microwave‐assisted extraction were researched by scanning electron microscopy and IR spectroscopy. All the results show that guanidinium ionic liquid based microwave‐assisted extraction has a huge potential in the extraction of bioactive compounds from complex samples.     

Ion‐pair switchable‐hydrophilicity solvent‐based homogeneous liquid–liquid microextraction for the determination of paraquat in environmental and biological samples before high‐performance liquid chromatography

An approach involving ion‐pair switchable‐hydrophilicity solvent‐based homogeneous liquid–liquid microextraction coupled to high‐performance liquid chromatography has been applied for the preconcentration and separation of paraquat in a real sample. A mixture of triethylamine and water was used as the switchable‐hydrophilicity solvent. The pH was regulated using carbon dioxide; hence the ratio of the ionized and non‐ionized form of triethylamine could control the optimum conditions. Sodium dodecyl sulfate was utilized as an ion‐pairing agent. The ion‐associate complex formed between the cationic paraquat and sodium dodecyl sulfate was extracted into triethylamine. The separation of the two phases was carried out by the addition of sodium hydroxide, which changed the ionization state of triethylamine. The effects of some important parameters on the extraction recovery were investigated. Under the optimum conditions (500 μL of the extraction solvent, 1 mg sodium dodecyl sulfate, 2.0 mL of 10 mol/L sodium hydroxide, and pH 4), the limit of detection and the limit of quantification were 0.2 and 0.5 μg/L, respectively, with preconcentration factor of 74. The precision (RSD, n  = 10) was  <5%. The recovery of the analyte in environmental and biological samples was in the range of 90.0–92.3%.     

Dispersive admicelle solid‐phase extraction based on sodium dodecyl sulfate coated Fe3O4 nanoparticles for the selective adsorption of three alkaloids in Gegen‐Qinlian oral liquid before high‐performance liquid chromatography

A novel dispersive admicelle solid‐phase extraction method based on sodium dodecyl sulfate‐coated Fe₃O₄ nanoparticles was developed for the selective adsorption of berberine, coptisine, and palmatine in Gegen‐Qinlian oral liquid before high‐performance liquid chromatography. Fe₃O₄ nanoparticles were synthesized by a chemical coprecipitation method and characterized by using transmission electron microscopy. Under acidic conditions, the surface of Fe₃O₄ nanoparticles was coated with sodium dodecyl sulfate to form a nano‐sized admicelle magnetic sorbent. Owing to electrostatic interaction, the alkaloids were adsorbed onto the oppositely charged admicelle magnetic nanoparticles. The quick separation of the analyte‐adsorbed nanoparticles from the sample solution was performed by using Nd‐Fe‐B magnet. Best extraction efficiency was achieved under the following conditions: 800 μL Fe₃O₄ nanoparticles suspension (20 mg/mL), 150 μL sodium dodecyl sulfate solution (10 mg/mL), pH 2, and vortexing time 2 min for the extraction of alkaloids from 10 mL of diluted sample. Four hundred microliters of methanol was used to desorb the alkaloids by vortexing for 1 min. Satisfactory extraction recoveries were obtained in the range of 85.9–120.3%, relative standard deviations for intra‐ and interday precisions were less than 6.3 and 10.0%, respectively. Finally, the established method was successfully applied to analyze the alkaloids in two batches of Gegen‐Qinlian oral liquids.     

Biosurfactant trehalose lipid‐enhanced ultrasound‐assisted micellar extraction and determination of the main antioxidant compounds from functional plant tea

Hydrosoluble trehalose lipid (a biosurfactant) was employed for the first time as a green extraction solution to extract the main antioxidant compounds (geniposidic acid, chlorogenic acid, caffeic acid, and rutin) from functional plant tea (Eucommia ulmoides leaves). Single‐factor tests and response surface methodology were employed to optimize the extraction conditions for ultrasound‐assisted micellar extraction combined with ultra‐high‐performance liquid chromatography in succession. A Box‐Behnken design (three‐level, three‐factorial) was used to determine the effects of extraction solvent concentration (1–5 mg/mL), extraction solvent volume (5–15 mL), and extraction time (20–40 min) at a uniform ultrasonic power and temperature. In consequence, the best analyte extraction yields could be attained when the trehalose lipid solution concentration was prepared at 3 mg/mL, the trehalose lipid solution volume was 10 mL and the extraction time was set to 35 min. In addition, the recoveries of the antioxidants from Eucommia ulmoides leaves analyzed by this analytical method ranged from 98.2 to 102%. These results indicated that biosurfactant‐enhanced ultrasound‐assisted micellar extraction coupled with a simple ultra‐high‐performance liquid chromatography method could be effectively applied in the extraction and analysis of antioxidants from Eucommia ulmoides leaf samples.     

Simultaneous determination of 106 pesticides in nuts by LC–MS/MS using freeze‐out combined with dispersive solid‐phase extraction purification

As a result of the low water content and high fat matrices in nuts, it is very difficult to simultaneously determine multi‐pesticides in trace levels. Here, a sample pretreatment method was developed in which, microwave‐assisted solvent extraction was firstly used to extract pesticides, and then a two‐step cleanup method was conducted combining freeze‐out with dispersive solid‐phase extraction to remove the lipidic matrix. By this way, 106 pesticides were simultaneously determined in the complicated nut sample by using an ultra‐high pressure liquid chromatography coupled with a tandem mass spectrometer. Average recoveries were 75.3–119.3% with relative standard deviations < 14% at three concentration levels. The limits of detection and quantification were in the ranges of 0.3–3.0 and 1.0–10.0 μg/kg, respectively. Furthermore, the method was successfully applied to the determination of pesticides in 180 commercial nut samples.     

Free amino acids,biogenic amines,and ammonium profiling in tobacco from different geographical origins using microwave‐assisted extraction followed by ultra high performance liquid chromatography

This work describes a rapid, stable, and accurate method for determining the free amino acids, biogenic amines, and ammonium in tobacco. The target analytes were extracted with microwave‐assisted extraction and then derivatized with diethyl ethoxymethylenemalonate, followed by ultra high performance liquid chromatography analysis. The experimental design used to optimize the microwave‐assisted extraction conditions showed that the optimal extraction time was 10 min with a temperature of 60°C. The stability of aminoenone derivatives was improved by keeping the pH near 9.0, and there was no obvious degradation during the 80°C heating and room temperature storage. Under optimal conditions, this method showed good linearity (R ² > 0.999) and sensitivity (limits of detection 0.010–0.081 μg/mL). The extraction recoveries were between 88.4 and 106.5%, while the repeatability and reproducibility ranged from 0.48 to 5.12% and from 1.56 to 6.52%, respectively. The newly developed method was employed to analyze the tobacco from different geographical origins. Principal component analysis showed that four geographical origins of tobacco could be clearly distinguished and that each had their characteristic components. The proposed method also showed great potential for further investigations on nitrogen metabolism in plants.     

Optimization of microwave‐assisted extraction followed by RP‐HPLC for the simultaneous determination of oleanolic acid and ursolic acid in the fruits of Chaenomeles sinensis

An optimized microwave‐assisted extraction (MAE) method and an efficient HPLC analysis method were developed for fast extraction and simultaneous determination of oleanolic acid and ursolic acid in the fruit of Chaenomeles sinensis. The open vessel MAE process was optimized by using a central composite experimental design. The optimal conditions identified were microwave power 600 W, temperature 52°C, solvent to material ratio 32 mL/g and extraction time 7 min. The results showed that MAE is a more rapid extraction method with higher yield and lower solvent consumption. The HPLC–photodiode array detection analysis method was validated to have good linearity, precision, reproduction and accuracy. Compared with conventional extraction and analysis methods, MAE–HPLC–photodiode array detection is a faster, convenient and appropriate method for determination of oleanolic acid and ursolic acid in the fruits of C. sinensis.     

Up‐and‐down shaker‐assisted ionic liquid‐based dispersive liquid—liquid microextraction of benzophenone‐type ultraviolet filters

Sun protection is an important part of our lives. UV filters are widely used to absorb solar radiation in sunscreens. However, excess UV filters constitute persistent groups of organic micropollutants present in the environment. An environmentally friendly ionic‐liquid‐based up‐and‐down shaker‐assisted dispersive liquid?liquid microextraction device combined with ultra‐performance liquid chromatography coupled with photodiode‐array detection has been developed to preconcentrate three UV filters (benzophenone, 2‐hydroxy‐4‐methoxybenzophenone, 2,2′‐dihydroxy‐4‐methoxybenzophenone) from field water samples. In this method, the optimal conditions for the proposed extraction method were: 40 μL [C₈MIM][PF₆] as extraction solvent and 200 μL methanol as disperser solvent were used to extract the UV filters. After up‐and‐down shaking for 3 min, the aqueous solution was centrifuged at 5000 rpm speed, then using microtube to collect the settled extraction solvent and using ultra‐performance liquid chromatography for further analysis. Quantification results indicated that the linear range was 2–1000 ng/mL. The LOD of this method was in the range 0.2–1.3 ng/mL with r² ≥ 0.9993. The relative recovery in studies of different types of field water samples was in the range 92–120%, and the RSD was 2.3–7.1%. The proposed method was also applied to the analysis of field samples.     

Simple magnetization of Fe3O4/MIL‐53(Al)‐NH2 for a rapid vortex‐assisted dispersive magnetic solid‐phase extraction of phenol residues in water samples

The present work describes a simple route to magnetize MIL‐53(Al)‐NH₂ sorbent for rapid extraction of phenol residues from environmental samples. To extend the applications and performances of the metal‐organic frameworks in the field of adsorption materials, we combined the properties of metal‐organic frameworks and magnetite to decrease the extraction time and simplify the extraction process as well. In this study, a simple and quick vortex‐assisted dispersive magnetic solid phase extraction method for the extraction of ten United States Environmental Protection Agency's priority phenols from water samples prior to analysis by high‐performance liquid chromatography with photodiode array detection was proposed. The developed method exhibits a rapid enrichment of the target analytes within 10 s for extraction and 10 s for desorption. Low detection limits of 1.8‐41.7 µg/L and quantitation limits of 6.0‐139.0 µg/L with the relative standard deviations for intra‐ and interday analyses less than 12% were achieved. Satisfactory recoveries in the range of 80‐111% with the relative standard deviations less than 11% demonstrated that Fe₃O₄/MIL‐53(Al)‐NH₂ is promising sorbent in the field of magnetic solid‐phase extraction for environmental samples.     

Application of ionic liquid‐based surfactants in the microwave‐assisted extraction for the determination of four main phloroglucinols from Dryopteris fragrans

An ionic liquid‐based surfactant combined with microwave‐assisted extraction method, followed by RP‐HPLC‐diode array detection (DAD) with a core shell column, was successfully applied in extracting and quantifying four major phloroglucinols from Dryopteris fragrans. Eight ionic liquids with different cation and anion were investigated, and 1‐octyl‐3‐methylimidazolium bromide presented the best relative extraction efficiency for four phloroglucinols. The optimum conditions of this method were as follows: ionic liquid concentration 0.75 M, liquid/solid ratio 12:1 mL/g, extraction time 7 min, extraction temperature 50°C, and irradiation power 600 W. The quality analytical parameters of the method were obtained based on the linearity, precision, accuracy, detection, and quantification limits. The recoveries were between 96.90 and 103.5% with standard deviations not higher than 4.7%. Compared with ionic liquid‐based heat reflux extraction, ultrasonic‐assisted extraction, negative‐pressure cavitation extraction, and conventional microwave‐assisted extraction, the relative extraction efficiencies of the proposed method for four phloroglucinols increased 1.5–40.4%. The method was successfully applied for the quantification of four major phloroglucinols from D. fragrans. All these results suggest that the developed method represents an excellent alternative for the extraction and quantification of phloroglucinols in other plant materials.     

Loading controlled magnetic carbon dots for microwave‐assisted solid‐phase extraction: Preparation,extraction evaluation and applications in environmental aqueous samples

An adsorbent of carbon dot@poly(glycidyl methacrylate)@Fe₃O₄ nanoparticles has been developed for the microwave‐assisted magnetic solid‐phase extraction of polycyclic aromatic hydrocarbons in environmental aqueous samples prior to high‐performance liquid chromatography with UV/visible spectroscopy detection. Poly(glycidyl methacrylate) was synthesized by atom transfer radical polymerization. The chain length and amount of carbon dots attached on them can be easily controlled through changing polymerization conditions, which contributes to tunable extraction performance. The successful fabrication of the nano‐adsorbent was confirmed by transmission electronic microscopy, Fourier transform infrared spectroscopy, Raman spectroscopy and vibrating sample magnetometry. The extraction performance of the adsorbent was evaluated by using polycyclic aromatic hydrocarbons as model analytes. The key factors influencing the extraction, such as microwave power, adsorption time, desorption time and desorption solvents were investigated in detail. Under the optimal conditions, the microwave‐assisted method afforded magnetic solid‐phase extraction with short extraction time, wide dynamic linear range (0.02–200 μg/L), good linearity (R² ≥ 98.57%) and low detection limits (20–90 ng/L) for model analytes. The adsorbent was successfully applied for analyzing polycyclic aromatic hydrocarbons in environmental aqueous samples and the recoveries were in the range of 86.0–124.2%. Thus, the proposed method is a promising candidate for fast and reliable preconcentration of trace polycyclic aromatic hydrocarbons in real water samples.     

Ionic‐liquid‐based ultrasound‐assisted extraction of isoflavones from Belamcanda chinensis and subsequent screening and isolation of potential α‐glucosidase inhibitors by ultrafiltration and semipreparative high‐performance liquid chromatography

The separation of a compound of interest from its structurally similar homologues to produce high‐purity natural products is a challenging problem. This work proposes a novel method for the separation of iristectorigenin A from its structurally similar homologues by ionic‐liquid‐based ultrasound‐assisted extraction and the subsequent screening and isolation of potential α‐glucosidase inhibitors via ultrafiltration and semipreparative high‐performance liquid chromatography. Ionic‐liquid‐based ultrasound‐assisted extraction was successfully applied to the extraction of tectorigenin, iristectorigenin A, irigenin, and irisflorentin from Belamcanda chinensis . The optimum conditions for the efficient extraction of isoflavones were determined as 1.0 M 1‐ethyl‐3‐methylimidazolium tetrafluoroborate with extraction time of 30 min and a solvent to solid ratio of 30 mL/g. Ultrafiltration with liquid chromatography and mass spectrometry was applied to screen and identify α‐glucosidase inhibitors from B. chinensis , followed by the application of semipreparative high‐performance liquid chromatography to separate and isolate the active constituents. Four major compounds including tectorigenin, iristectorigenin A, irigenin, and irisflorentin were screened and identified as α‐glucosidase inhibitors, and then the four active compounds abovementioned were subsequently isolated by semipreparative high‐performance liquid chromatography (99.89, 88.97, 99.79, and 99.97% purity, respectively). The results demonstrate that ionic liquid extraction can be successfully applied to the extraction of isoflavones from B. chinensis .     

Optimization of extraction for Anemarrhena asphodeloides Bge. using silica gel‐based vortex‐homogenized matrix solid‐phase dispersion and rapid identification of antioxidant substances

A novel and simple method was established for the extraction and determination of seven compounds in Anemarrhena asphodeloides Bge. using silica gel‐based vortex‐homogenized matrix solid‐phase dispersion and ultra‐high performance liquid chromatography quadrupole‐time of‐flight mass spectrometer. The conditions for the extraction were optimized. Silica gel was used as the dispersant, 50% methanol–water was selected as an elution solvent and the grinding time was 3 min. Compared with the traditional ultrasonic‐assisted extraction, the developed method was rapid and efficient. In order to screen potential antioxidants, extract dealing with the optimized method was applied to a polyamide chromatography column and a D‐101 macroporous resin column. Fr.2.2 showed the highest antioxidant activities with the most content of flavonoid. A total of 25 peaks were identified from the active fraction. A 2,2′‐diphenyl‐1‐picrylhydrazyl ultra‐high performance liquid chromatography coupled with mass spectrometry approach was adopted for the rapid and exact screening and identification of antioxidant compounds. It indicated that flavonoids exhibited potential antioxidant activities. The antioxidant activities of nine monomeric compounds in vivo were tested. Structure–activity relationships were discussed. Five flavonoids with the concentration of 500 µg/mL would reduce the oxidative stress of PC12 cells that were induced with 2,2′‐azobis[2‐methylpropionamidine] dihydrochloride.     

Sodium dodecyl sulfate sensitized switchable solvent liquid‐phase microextraction for the preconcentration of protoberberine alkaloids in Rhizoma coptidis

A sodium dodecyl sulfate sensitized switchable solvent liquid‐phase microextraction method was developed and applied to the preconcentration of active alkaloids in Rhizoma coptidis followed by high performance liquid chromatography determination. Before extraction, nonionic triethylamine was converted to its cationic form in the presence of carbon dioxide. Then, the ionic solvent carrying target analytes was once more reverted to its nonionic form by adding sodium hydroxide, as well as phase separation and analytes enrichment were realized simultaneously. Several parameters affecting the approach, such as concentration of sodium dodecyl sulfate, extraction solvent volume, sodium hydroxide concentration, sample phase pH, injection solvent type, and extraction time, were investigated and optimized. The possible microextraction mechanism of double micelle supramolecular inclusion was explored. Under the optimum conditions, the enrichment factors of four protoberberine alkaloids were from 101.8 to 152.0. The linear ranges (with r² ≥ 0.990) were 0.032–4.23, 0.031–4.33, 0.0026–10.04, and 0.0013–4.13 μg/mL for epiberberine, coptisine, palmatine, and berberine, respectively. The detection limits were in the range of 0.16–0.32 ng/mL. Satisfactory accuracies (recoveries 98.8–104.6%) and precisions (RSDs 1.9–10.9%) were also obtained. The results showed that the approach is rapid, effective, eco‐friendly, and easy‐to‐handle for the enrichment and detection of active alkaloids in Rhizoma coptidis.     

Optimized determination of polybrominated diphenyl ethers by ultrasound‐assisted liquid–liquid extraction and high‐performance liquid chromatography

A method based on ultrasound‐assisted liquid–liquid extraction and high‐performance liquid chromatography has been optimized for the determination of six polybrominated diphenyl ether congeners. The optimal condition relevant to the extraction was first investigated, more than 98.7 ± 0.7% recovery was achieved with dichloromethane as extractant, 5 min extraction time, and three cycles of ultrasound‐assisted liquid–liquid extraction. Then multiple function was employed to optimize polybrominated diphenyl ether detection conditions with overall resolution and chromatography signal area as the responses. The condition chosen in this experiment was methanol/water 93:7 v/v, flow rate 0.80 mL/min, column temperature 30.0°C. The optimized technique revealed good linearity (R² > 0.9962 over a concentration range of 1–100 μg/L) and repeatability (relative standard deviation < 6.3%). Furthermore, the detection limit (S/N = 3) of the method were ranged from 0.02 to 0.13 μg/L and the quantification limit (S/N = 10) ranged from 0.07 to 0.35 μg/L. Finally, the proposed method was applied to spiked samples and satisfactory results were achieved. These results indicate that ultrasound‐assisted liquid–liquid extraction coupled with high‐performance liquid chromatography was effective to identify and quantify the complex polybrominated diphenyl ethers in effluent samples.     

Rapid and sensitive determination of major polyphenolic components in Euphoria longana Lam. seeds using matrix solid‐phase dispersion extraction and UHPLC with hybrid linear ion trap triple quadrupole mass spectrometry

A rapid and sensitive method for the extraction and determination of four major polyphenolic components in Euphoria longana Lam. seeds is presented for the first time based on matrix solid‐phase dispersion extraction followed by ultra high performance liquid chromatography with hybrid triple quadrupole linear ion trap mass spectrometry. Matrix solid‐phase dispersion method was designed for the extraction of Euphoria longana seed constituents and compared with microwave‐assisted extraction and ultrasonic‐assisted extraction methods. An Ultra high performance liquid chromatography with hybrid triple quadrupole linear ion‐trap mass spectrometry method was developed for quantitative analysis in multiple‐reaction monitoring mode in negative electrospray ionization. The chromatographic separation was accomplished using an ACQUITY UPLC BEH C₁₈ (2.1 mm × 50 mm, 1.7 μm) column with gradient elution of 0.1% aqueous formic acid and 0.1% formic acid in acetonitrile. The developed method was validated with acceptable linearity (r² > 0.999), precision (RSD ≤ 2.22%) and recovery (RSD ≤ 2.35%). The results indicated that matrix solid‐phase dispersion produced comparable extraction efficiency compared with other methods nevertheless was more convenient and time‐saving with reduced requirements on sample and solvent volumes. The proposed method is rapid and sensitive in providing a promising alternative for extraction and comprehensive determination of active components for quality control of Euphoria longana products.     

Microwave‐assisted extraction followed by RP‐HPLC for the simultaneous extraction and determination of forsythiaside A,rutin, and phillyrin in the fruits of Forsythia suspensa

An optimized microwave‐assisted extraction (MAE) method and RP‐HPLC method were developed for the simultaneous extraction and determination of rutin, forsythiaside A, and phillyrin in the fruits of Forsythia suspensa. The key parameters of the open‐vessel MAE process were optimized. A mixed solvent of methanol and water (70:30, v/v) was most suitable for the simultaneous extraction of the three components. The sample was soaked for 10 min before extraction. The optimized conditions were: microwave power 400 W, temperature 70°C, solvent‐to‐material ratio 30 mL/g, and extraction time 1 min. Compared to conventional extraction methods, the proposed method can simultaneously extract the three components in high yields and was proved to be a more rapid method with a lower solvent consumption. The optimized HPLC–photodiode array detection analysis was validated to have good linearity, precision, accuracy, and sensitivity. The developed MAE followed by RP‐HPLC is a fast and appropriate method for the simultaneous extraction and determination of rutin, forsythiaside A, and phillyrin in the fruits of F. suspensa.     

Rapid and cost‐effective method for the simultaneous quantification of seven alkaloids in Corydalis decumbens by microwave‐assisted extraction and capillary electrophoresis

A rapid and cost‐effective method based on microwave‐assisted extraction followed by capillary electrophoresis was developed for simultaneous quantification of seven alkaloids in Corydalis decumbens for the first time. The main parameters affecting microwave‐assisted extraction and capillary electrophoresis separation were investigated and optimized. The optimal microwave‐assisted extraction was performed at 40°C for 5 min using methanol/water (90:10, v/v) as the extracting solvent. Electrophoretic separation was achieved within 15 min using an uncoated fused‐silica capillary (50 μm internal diameter and 27.7 cm effective length) and a 500 mM Tris buffer containing 45% v/v methanol (titrated to pH^* 2.86 with H₃PO₄). The developed method was successfully applied to the quantification of seven alkaloids in Corydalis decumbens obtained from different regions of China. The combination of microwave‐assisted extraction with capillary electrophoresis was an effective method for the rapid analysis of the alkaloids in Corydalis decumbens .