Dispersive Solid-Phase Extraction Clean-up Combined with Dispersive Liquid�CLiquid Microextraction for the Determination of Neonicotinoid Insecticides in Vegetable Samples by High-Performance Liquid Chromatography

Dispersive solid-phase extraction (DSPE) clean-up combined with dispersive liquid–liquid microextraction (DLLME) has been developed as a new approach for the extraction of neonicotinoid insecticides in vegetable samples prior to high-performance liquid chromatography with diode array detection. In the DSPE–DLLME method, neonicotinoid insecticides were first extracted with acetonitrile from vegetable samples, followed by clean-up by a DSPE with primary secondary amine and multi-walled carbonnanotubes as sorbents. A 2.5-mL aliquot of the resulting extract was then added into a centrifuge tube containing 10 mL of water, 0.8 g NaCl, and 200-μL chloroform (as the extraction solvent) for DLLME procedure. Under the optimum conditions, the enrichment factors for the compounds were in the range between 110 and 243. The linearity of the method was in the range from 5.0 to 300 ng g⁻¹ with the correlation coefficients (r) ranging from 0.9989 to 0.9998. The detection limits of the method were 0.5–1.0 ng g⁻¹. The repeatability of the method expressed as the relative standard deviations by five parallel experiments at the concentration levels of 10 and 50 ng g⁻¹ each of the neonicotinoid insecticides in tomato or cucumber samples varied from 3.6% to 5.8%. The developed method has been successfully applied for the analysis of target neonicotinoid insecticides (acetamiprid, imidacloprid, thiacloprid, and thiamethoxam) in tomato and cucumber samples. The recoveries of the method for the target neonicotinoid insecticides from the vegetable samples at spiking levels of 10.0 and 50.0 ng g⁻¹ were in the range between 84.6% and 97.5% (n = 5).     

Dispersive Liquid–Liquid Microextraction Followed by Capillary High-Performance Liquid Chromatography for the Determination of Six Sulfonylurea Herbicides in Fruit Juices

In this study a simple, rapid, and efficient method has been developed for the determination of six sulfonylurea herbicides (SUHs): triasulfuron, metsulfuron-methyl, chlorsulfuron, flazasulfuron, chlorimuron-ethyl, and primisulfuron-methyl in commercial grape and apple juice samples, using dispersive liquid–liquid microextraction coupled with capillary high-performance liquid chromatography with diode array detection. Various parameters that influence the extraction efficiency, such as the type and volume of extraction and disperser solvents, sample pH, and salt addition, were investigated and optimized. Under the optimum conditions, limits of detection and quantification of the method were in the ranges of 2–9 and 8–29 μg L^?1, respectively, lower than the maximum residue limits set by the European Union for the raw fruits, such as grape and apple. The intra- and inter-day relative standard deviations varied from 1.0 to 8.2 and 1.8 to 9.8 %, respectively, with recoveries between 72.0 and 109.5 % for commercial grape (both white and red) and apple juice samples, showing satisfactory accuracy for the determination of SUHs in fruit juices.     

Determination of Sulfite in Water and Dried Fruit Samples by Dispersive Liquid–Liquid Microextraction Combined with UV–Vis Fiber Optic Linear Array Spectrophotometry

A simple and rapid dispersive liquid?Cliquid microextraction (DLLME) method was applied to preconcentrate sulfite ions from aqueous samples as a prior step to its determination by fiber optic-linear array detection spectrophotometry. The procedure is based on the color reaction of sulfite with o-phthaldialdehyde (OPA) in the presence of ammonia to form isoindole and extraction of the formed isoindole derivative using the DLLME technique. The conditions for the microextraction performance were investigated and optimized. The calibration graph was linear in the range of 2?C100???g?L^?1with a detection limit of 0.2???g?L^?1. The relative standard deviation for five replicate measurements of 10 and 50???g?L^?1of sulfite were 2.8 and 2.0?%, respectively. Under the optimized conditions, the enrichment factor of ~133 was obtained from a sample volume of 10?mL. The proposed method was successfully applied to the sulfite determination in drinking water and in food samples.     

Dispersive Liquid–Liquid Microextraction Followed by Magnetic Solid-Phase Extraction for Determination of Four Parabens in Beverage Samples by Ultra-performance Liquid Chromatography Tandem Mass Spectrometry

In this study, a two-step extraction technique was developed for extraction and preconcentration of parabens from beverage samples using ionic liquid dispersive liquid–liquid microextraction (IL-DLLME) and magnetic solid-phase extraction (MSPE). In this IL-DLLME followed by MSPE method, ionic liquid (IL, 1-octyl-3-methylimidazolium hexafluorophosphate) formed hydrophobic microdroplets in beverage samples as an extractant of parabens; after the IL-DLLME process was completed, graphene modified Fe₃O₄ nanoparticles (Fe₃O₄@G) were placed to adsorb and isolate IL from the sample solution. After the supernatant was carefully moved, acetonitrile was added to elute the IL containing parabens from Fe₃O₄@G. The experimental variables affecting the extraction procedure have been systematically studied. Under optimal conditions, the detection limits were less than 1.53 ng/mL and the linear detection ranges were 2–500 ng/mL (R ² ≥ 0.998) for these analytes. The recoveries for spiked samples were 58.8–89.2% and satisfactory precision (RSD ≤ 4.8%) were obtained.     

Surfactant–Solvent-Based Quaternary Component Emulsification Microextraction Followed by High-Performance Liquid Chromatography for the Simultaneous Analysis of Benzimidazole Anthelmintics in Milk Samples

A simple surfactant-solvent-based quaternary component emulsification microextraction (SSEME) method combined with high-performance liquid chromatography–photodiode array detection has been developed for the extraction, preconcentration, and determination of four benzimidazole anthelmintic (i.e., oxfendazole, mebendazole, albendazole, and fenbendazole) residues in milk samples. The quaternary component solvent of SSEME carried out in 10 mL aqueous solution were Triton X-114 (emulsifier or carrier), acetonitrile (disperser solvent), and 1-octanol (extraction solvent). The surfactant has an important role in the enhancement of the extraction efficiency of the high polar analytes. For milk sample analyses, linearity was obtained in the range of 10–200 μg/L with the determination coefficients (R ²) higher than 0.996. Preconcentration factor was obtained in the range of 21–38, corresponding to limits of detection in the range of 2.6–9.9 μg/L. Intra-day (n?=?6) and inter-day (n?=?6?×?3) precisions in the sample studied were obtained with relative standard deviation below 8.8 %. The recoveries for the spiked target anthelmintics at different concentrations (25, 50, 100, and 150 μg/L) were obtained in the range 80.1–114.1 %. The proposed SSEME method has been demonstrated that is simple, effective, and reliable for the analysis of analytes in the samples studied and can be used as an alternative green analytical technique for benzimidazole analysis.     

Development of a Dispersive Liquid–Liquid Microextraction Method for the Determination of α-Tocopherol in Pigmented Wheat by High-Performance Liquid Chromatography

A dispersive liquid–liquid microextraction (DLLME) method coupled to high-performance liquid chromatography was developed for the analysis of α-tocopherol in grain samples. The DLLME parameters including the type and volume of extractants, the volume of disperser and the addition of salt were examined. The optimized DLLME procedure consisted in the formation of a cloudy solution promoted by the fast addition to the sample (5 mL of saponified sample solution diluted with 5 mL of water) of a mixture of carbon tetrachloride (extraction solvent, 80 μL) and ethanol (dispersive solvent, 200 μL) without the addition of salt, followed by shaking for 5 min and centrifuging for 3 min at 5,000 rpm. Intra- and inter-day repeatability expressed as % RSD were 3.5 and 7.6 %, respectively. The limit of detection and the limit of quantification were 1.9 and 6.3 μg?L^?1. The comparison of this method with the national standardized extraction method, supercritical carbon dioxide extraction, accelerated solvent extraction, and conventional heat-reflux extraction indicates that the DLLME was accurate (no significant differences at the 0.05 % probability level), high efficient, low organic solvent-consuming, and low cost. This procedure was successfully applied to 42 samples of 14 types of purple wheat, for which the content of α-tocopherol exhibited a significantly negative correlation with the pigment content measured by a spectrophotometer. The recovery rates ranged from 90.5 to 103.7 %.     

Optimized Dispersive Liquid–Liquid Microextraction and Determination of Sorbic Acid and Benzoic Acid in Beverage Samples by Gas Chromatography

A new rapid method for direct determination of trace levels of sorbic and benzoic acids was developed by dispersive liquid–liquid microextraction and gas chromatography with flame ionization detection. In the proposed approach, the separation procedure of sorbic and benzoic acids was performed on a general chromatographic column without any prior derivatization processes. Some effective parameters on the microextraction recovery were studied and optimized utilizing multilevel factorial and central composite experimental designs. The best concurrent extraction efficiency acquired using ethanol and chloroform as dispersive and extraction solvents. Central composite design (CCD) resulted in the optimized values of microextraction parameters as follows: 1.0 mL of dispersive and 0.1 mL of extraction solvents, ionic salt concentration of 50 g?L^?1 at pH 4. Under optimum conditions, the calibration curve was linear over the range 0.5–20 mg L^?1. Relative standard deviation was 11% and 13% for five repeated determinations for sorbic and benzoic acids, respectively. Limits of detection were acquired as 0.2 mg L^?1 for sorbic acid and 0.5 mg L^?1 for benzoic acid. The average recoveries were 31% and 39% for sorbic and benzoic acids, respectively. The method was successfully applied to the determination of sorbic and benzoic acids as preservatives in beverage samples.     

Application and Optimization of Microwave-Assisted Extraction and Dispersive Liquid–Liquid Microextraction Followed by High-Performance Liquid Chromatography for the Determination of Oleuropein and Hydroxytyrosol in Olive Pomace

In the present study, a new method based on microwave-assisted extraction and dispersive liquid–liquid microextraction (MAE–DLLME) followed by high-performance liquid chromatography (HPLC) was proposed for the separation and determination of oleuropein (Ole) and hydroxytyrosol (HyT) from olive pomace samples. The effective factors in the MAE–DLLME process such as microwave power, extraction time, the type and volume of extraction, and dispersive solvents were studied and optimized with the aid of response surface methodology (RSM) based on a central composite design (CCD) to obtain the best condition for Ole and HyT extraction. At the optimized conditions, parameter values were 220 W microwave power, 12 min extraction time, 60 μL extracting solvent, and 500 μL dispersive solvent. The calibration graphs of the proposed method were linear in the range of 10–500,000 μg L^?1, with the coefficient of determination (R²) higher than 0.99 for Ole and HyT. Repeatability of the method, described as the relative standard deviation (RSD), was 4.12–5.63% (n?=?6). The limits of detection were 35 and 20 μg L^?1 for Ole and HyT, respectively. The recoveries of these compounds in the spiked olive pomace sample were from 93 to 98%. The proposed method, MAE–DLLME–HPLC–UV, was an accurate, rapid, and reliable method when compared with previous methods.     

Ionic Liquid-Based Dispersive Liquid–Liquid Microextraction Following High-Performance Liquid Chromatography for the Determination of Fungicides in Fruit Juices

This paper described an ionic liquid-based dispersive liquid–liquid microextraction (IL-DLLME) combined with high-performance liquid chromatography (HPLC) method to determine fungicides in fruit juices. In this method, 1-hexyl-3-methyli-midazolium hexafluorophosphate (HMIMPF₆) was used as extraction solvent, which dispersed into the fruit juices under vigorously shaking with the vortex. The effects of experimental parameters, such as extraction solvent volume, disperser solvent and its volume, vortex time, centrifugation time, sample pH, on the extraction efficiency were investigated. Under the optimum conditions, the linear correlation coefficients ranged from 0.9902 to 0.9979 for concentration levels of 0.02–2 mg l^?1, the extraction recoveries were ranged 66.2–92.9 % except pyrimethanil (39.5–44.6 %), The relative standard deviations (RSDs; n?=?6) ranged from 2.2 % to 11.6 %, and the limits of detection (LODs) for the fungicides were between 3.1 and 10.2 μg l^?1. Two real samples including apple and grape juices, spiked at two concentration levels were analyzed and yielded recoveries ranging from 71.3–93.1 % and 65.4–87.7 %, respectively.     

Determination of Triazoles in Tea Samples Using Dispersive Solid Phase Extraction Combined with Dispersive Liquid–Liquid Microextraction Followed by Liquid Chromatography–Tandem Mass Spectrometry

In this study, dispersive solid phase extraction (DSPE) combined with dispersive liquid–liquid microextraction (DLLME) method was developed for the determination of triazole fungicide residues in tea samples. DSPE with ODS C₁₈, primary secondary amine, and florisil as sorbents was applied to clean up and minimize matrix interference from tea samples; it was followed with the enrichment of target compounds in the DLLME procedure and detection with liquid chromatography–tandem mass spectrometry (LC-MS/MS). The effects of various experimental parameters on the DSPE and DLLME procedures were studied systematically, such as the kinds and volume of sorbents, extraction and dispersive solvents, and extraction time. Under optimum conditions, the method was validated in a tea matrix. The matrix-matched calibration curves of three triazoles had good linearity in the range of 0.0125–50 μg kg^?1, and the linear regression coefficients (r) ranged from 0.9998 to 0.9999. The limits of quantification (S/N?=?10) for penconazole, tebuconazole, and triadimenfon were 4.0, 7.8, and 31.6 ng kg^?1, respectively. The intra-day and inter-day relative standard deviations varied from 3.6 to 18.6 %. Recoveries in three concentration levels were between 91 and 118 %. The obtained results show that the proposed DSPE-DLLME-LC-MS method has the potential to analyze trace fungicides in a complex sample matrix.     

Analysis of Pesticides in Tomato Combining QuEChERS and Dispersive Liquid–Liquid Microextraction Followed by High-Performance Liquid Chromatography

A new sample preparation procedure combining QuEChERS and dispersive liquid–liquid microextraction (DLLME) was optimized for the determination at trace levels of 13 pesticides from different chemical families (i.e. 2,4-D, acetamiprid, bentazone, cymoxanil, deltamethrin, dicamba, diuron, foramsulfuron, mesotrione, metalaxyl-M, methomyl, pyraclostrobin and tembotrione) in tomato by high-performance liquid chromatography with diode array detection. Target pesticides from tomato samples were isolated by liquid partitioning with acetonitrile and salts and cleaned up by dispersive solid-phase extraction (d-SPE); the analytes were concentrated in trichloromethane by the DLLME procedure. The disperser solvent from DLLME was used at the same time as carrier of analytes form extraction in QuEChERS method. The main factors affecting sample cleanup by d-SPE in QuEChERS and DLLME yield were optimized by means of an experimental design. Under the optimum conditions, good linearity was obtained, the recoveries of pesticides in tomato samples at spiking levels between 0.01 and 1.00 mg/kg ranged from 86 to 116 % (for foramsulfuron and cymoxanil, respectively). Precision was within 15.0 % (RSD) except at the LQ for tembotrione, which was 17.4 %. Limits of quantification achieved (ranging from 0.0058 to 0.15 mg/kg) were below the maximum residue limits established by the European Union.     

A New Extraction Method for the Determination of Oxytocin in Milk by Enzyme Immune Assay or High-Performance Liquid Chromatography: Validation by Liquid Chromatography–Mass Spectrometry

There has been a controversy regarding the use of exogenous oxytocin (OT) in milking cattle which may have toxicological consequences during nonphysiological exposure. In the present study, a new sensitive extraction method for OT was developed followed by enzyme immune assay (EIA) or high-performance liquid chromatography (HPLC) analysis. The extraction of OT in milk involves two steps: (1) TCA precipitation of milk proteins and (2) solid-phase extraction (SPE) cleanup process. Without these steps, analysis of OT in milk was not possible. Utilizing EIA as a quantitative tool the limit of detection (LOD) and limit of quantitation (LOQ) were found to be 7.74 and 10.3 pg?ml^?1, precision in terms of intra- and interday coefficient of variation was below 13 % (%RSD, N?=?8), while percent recoveries were between 85 and 92 %. Utilizing UV-HPLC, the LOD, LOQ, precision, and recovery values were found to be 4.1 ng?ml^?1, 9.8 ng?ml^?1, 2–10 %, and 84–91 %, respectively. OT was found to be stable against adverse temperature (up to 100 °C) and pH (2 to 10) and simulated gastric fluid digestibility assay. Four milk samples collected from the market were analyzed, which showed that TCA precipitation and SPE steps are mandatory and the results were validated by LC-MS showing mass ion peak at 1 kD.     

Vortex-Assisted Liquid–Liquid Microextraction Combined with HPLC for the Simultaneous Determination of Five Phthalate Esters in Liquor Samples

A vortex-assisted liquid–liquid microextraction (VALLME) method using hexanoic acid as extractant followed by high-performance liquid chromatography–diode array detection was developed for the extraction and determination of five phthalate esters (PAEs) including bis-methylglycol ester (DMEP), benzyl butyl phthalate (BBP), dicyclohexyl phthalate (DCHP), di-n-butyl phthalate (DBP), and di-n-octyl phthalate (DNOP) from liquor samples. In this method, hexanoic acid was employed as extraction solvent, because its density is lower than water. And vortex mixing was utilized as a mild emulsification procedure to reduce emulsification time and improve the effect of extraction. Under the studied conditions, five phthalate esters were successfully separated within 20 min and the limits of detection were 2.3 ng mL^?1 for DMEP, 1.1 ng mL^?1 for BBP, 1.9 ng mL^?1 for DCHP, 1.2 ng mL^?1 for DBP, and 1.5 ng mL^?1 for DNOP, respectively. Recoveries of the PAEs spiked into liquor samples were ranged from 89 to 93 %. The precisions of the proposed method were varied from 1.6 to 2.6 % (RSD). The VALLME method has been proved to have the potential to be applied to the preconcentration of the target analytes. Moreover, the method is simple, high sensitivity, consumes much less solvent than traditional methods and environmental friendly.     

Dispersive Liquid–Liquid Microextraction Combined With Micellar Electrokinetic Chromatography for the Determination of Some Photoinitiators in Fruit Juice

A fast and simple technique composed of dispersive liquid–liquid microextraction (DLLME) and micellar electrokinetic chromatography (MEKC) with diode array detector (DAD) was developed for the determination of multi-photoinitiators in fruit juice. Seven photoinitiators were separated in MEKC using a 25 mM borate buffer of pH 8.0, containing 24 mM sodium dodecyl sulfate (SDS), 10 mM β-cyclodextrin (β-CD), and 12.5 % acetonitrile (v/v). A CD-modified MEKC made this method more suitable for the determination of isopropylthioxanthone (ITX) isomers including 2-IXT and 4-ITX than the recently prescribed methods. A DLLME procedure was used as an offline preconcentration strategy. The satisfactory recoveries obtained by DLLME spiked at two spiked levels ranged from 85.6 to 124.7 % with relative standard deviations (RSDs) below 14 %. The limits of quantification (LOQs) ranged from 2.1 to 6.0 μg kg^?1.     

Determination of Benzalkonium Homologues and Didecyldimethylammonium in Powdered and Liquid Milk for Infants by Hydrophilic Interaction Liquid Chromatography–Mass Spectrometry

In this study, a hydrophilic interaction liquid chromatography–mass spectrometry (HILIC-MS/MS) method for the determination of benzalkonium (BAC) homologues and didecyldimethylammonium (DDAC) was developed. A satisfactory chromatographic separation of BAC homologues and DDAC was achieved using, as mobile phase, acetonitrile–aqueous 50 mM ammonium formate (pH 3.2) (93?+?7 v/v) at 0.3 mL min^?1. The elution order of BAC homologues was from benzyldimethylhexadecylammonium chloride (C₁₆-BAC) to benzyldimethyldecylammonium chloride (C₁₀-BAC), the exact opposite with respect to separation using reversed liquid chromatography. The instrumental method was successfully applied to powdered and liquid milk for infants (about 50 samples). From powdered milk samples, BAC and DDAC were extracted using 5 % formic acid in methanol for 60 min at 60 °C in an ultrasonic bath; after dilution with water and 5 % NH₄OH solution, a purification step using a weak cationic exchange column was performed. Satisfactory limit of detections (LODs) were achieved, below 1.0 μg kg^?1 and 0.05 μg L^?1 for powdered and liquid milk for infants, respectively. No sample was free of BAC homologues and DDAC, and in one powdered milk sample, the contamination level exceeded 500 μg kg^?1, the maximum level recommended by the Standing Committee on the Food Chain and Animal Health for food and feed.     

Ultrasound-Assisted Extraction Followed by Solid-Phase Extraction Followed by Dispersive Liquid–Liquid Microextraction for the Sensitive Determination of Diazinon and Chlorpyrifos in Rice

Selectivity of solid-phase extraction (SPE) was combined with the concentration power of dispersive liquid–liquid microextraction (DLLME) to obtain a sensitive, low solvent consumption method for high-performance liquid chromatography determination of diazinon and chlorpyrifos in rice. In this method, rice samples were extracted by ultrasound-assisted extraction followed by SPE. Then, the SPE eluent was used as a disperser solvent in the next dispersive liquid-liquid microextraction step for further purification and enrichment of diazinon and chlorpyrifos. Under the optimal conditions, the linear range was from 5.0 to 250 μg kg^?1 for diazinon and from 2.5 to 250 μg kg^?1 for chlorpyrifos. Limits of detection of diazinon and chlorpyrifos were 1.5 and 0.7 μg kg^?1, respectively. Limits of quantitation of diazinon and chlorpyrifos were 5.5 and 3.0 μg kg^?1, respectively. The precisions and recoveries also were investigated by spiking 10 μg kg^?1 concentration in rice. The recoveries obtained were over 90 % with relative standard deviation (RSD%) below 9.0 %. The new approach was utilized to successfully detect trace amounts of diazinon and chlorpyrifos in different Iranian rice samples.     

Aluminium and Its Complexes in Teas and Fruity Brew Samples,Speciation and Ions Determination by Ion Chromatography and High-Performance Liquid Chromatography–Fluorescence Analytical Methods

The paper presents results of aluminium determination in samples of black and fruit teas. Total aluminium concentration was determined along with the concentration of aluminium in a cup of tea in tea samples in two price groups (>1€ and <1€). Based on the conducted study, no differences were found in aluminium concentration in black and fruit teas depending on the price group. Developed ion chromatography method was applied to determine inorganic and organic ions in tea samples, especially those which may form complexes with aluminium: fluoride, sulphate, oxalate and citrate ions. Analysis by this method using ion chromatography allowed for the determination of 12 anions: F^?, HCOO^?, CH₃COO^?, NO₂ ^?, Br^?, NO₃ ^?; Cl^?, CH₂(COO)₂ ^2?, SO₄ ^2?, C₂O₄ ^2?, PO₄ ^3? and C₃H₅O(COO)₃ ^3? in the time of 40 min. Speciation analysis of aluminium was performed in optimised HPLC-fluorescence analytical system (with Lumogallion as a post-column reagent). It was observed that organic aluminium complexes are quickly degraded to form Al³⁺ which is the reason why speciation analysis in tea samples does not provide the full image of speciation distribution. Nevertheless, this developed method was successfully used in the determination of aluminium complexes with fluorides in tea samples.     

Novel Binary Solvents-Dispersive Liquid—Liquid Microextraction (BS-DLLME) Method for Determination of Patulin in Apple Juice Using High-Performance Liquid Chromatography

A simple and rapid binary solvents-based dispersive liquid–liquid microextraction (BS-DLLME) method has been developed for determination of patulin (PAT) in apple juice followed by high-performance liquid chromatography. This method involves the use of an appropriate mixture of miscible binary extraction solvents and disperser solvent to form fine droplets of extractant in a sample solution. Parameters affecting extraction efficiency such as the type and volume of high-density extraction solvent, the volume of ethyl acetate, the kind and volume of disperser solvent, and salt addition were investigated and optimized. The detection and quantification limits were 2.0 and 10.0 μg L^?1, respectively. The relative standard deviation for five measurements of 25 μg L^?1 of PAT was 3.8 %. The relative recoveries of PAT from apple juice samples at spiking levels of 25, 50, and 75 ng mL^?1 were in the range of 91.3–95.2 %.     

Ionic Liquid-Based Vortex-Assisted Liquid–Liquid Microextraction for Simultaneous Determination of Neonicotinoid Insecticides in Fruit Juice Samples

A simple, rapid, and effective method was developed for preconcentration of neonicotinoid insecticides including clothianidin, imidacloprid, acetamiprid, and thiacloprid in fruit juice samples. Room-temperature ionic liquids [C₄MIM][PF₆] can be used as green extractant phases in vortex-assisted liquid–liquid microextraction (VALLME), being compatible with high-performance liquid chromatographic systems. The effect of extraction parameters, including the addition of salt, volume of (C₄MIM)(PF₆), vortex time, and centrifugation time is identified as the key parameters of the method. Under the selected conditions, the high enrichment factors of 100 could be achieved with the limit of detection in the range of 0.25–0.30 ng mL^?1 and with the relative standard deviations of lower than 2.68 and 5.38 % for retention time and peak area, respectively. The proposed method was applied to the analysis of fruit juice samples, and the recoveries of the analytes ranged from 95 to 108 % and relative standard deviations were lower than 7 %. The developed method proposes advantages in reduction of the exposure danger to toxic organic solvents used in the conventional liquid–liquid extraction, simplicity of the extraction processes, rapidity, and sensitivity improvement.     

Determination of the Nicotine Content in Solanaceae Vegetables by Solid-Phase Extraction Coupled with Ultra High-Performance Liquid Chromatography–Tandem Mass Spectrometry

A validated method based on solid-phase extraction and ultra high-performance liquid chromatography–triple quadrupole tandem mass spectrometry, with electrospray ionization operated in the positive ion mode and multiple reaction monitoring, was developed for the determination of nicotine in Solanaceae vegetables. Sample preparation involved liquid–solid extraction, centrifugation, filtration, and solid-phase extraction. Two kinds of solid-phase extraction adsorbents, based on different retention mechanisms, were investigated. Relatively higher recoveries were obtained with a hydrophilic–lipophilic-balanced cartridge. A deuterated internal standard was used for quantification. The limit of quantification (LOQ) of nicotine in different vegetables was found to be between 0.07 and 0.5 μg/kg. The nicotine levels in the vegetable samples were above the LOQs. The method described here is thus suitable for the analysis of large sample batches, because it provides accurate quantification, high sensitivity and rapid chromatographic separation with facile preparation. The solid-phase extraction cartridges and organic solvents used in this work are easy to obtain, enabling the application of this method in most analytical laboratories.