Rapid Method For Simultaneous Determination Research Articles

Development of a Rapid Method for Simultaneous Determination of Pesticides in Plant Oil Using GC-MS/MS

Development of a Rapid Method for Simultaneous Determination of Pesticides in Plant Oil Using GC-MS/MS

A high-throughput method for the determination of 14 UV-filters in human plasma by LC-MS/MS: Minimize interferences from proteins and phospholipids in the matrix

Accurate monitoring of UV-filters exposure levels in human plasma is a challenge because of the significant differences in the physicochemical properties of UV-filters, as well as the matrix effect caused by abundant proteins and phospholipids in plasma. Therefore, an effective and rapid method for simultaneous determination of 14 UV-filters in human plasma using protein precipitation-solid phase extraction (SPE) coupled with liquid chromatography tandem mass spectrometry (LC-MS/MS) was developed. Acetonitrile with 0.1 % formic acid and 10 % isopropanol (v/v) were used as mobile phases. A gradient elution on an ACQUITY UPLC BEH-C18 column at 30 °C and 0.3 mL/min flow rate was applied for separation. The electrospray ionization positive or negative modes were selected to determine the corresponding analyte to increase selectivity and sensitivity. Results showed that acetonitrile-tetrahydrofuran (v/v, 8:2) as the extraction solvent can effectively precipitate protein in plasma and improve the solubility of UV-filters. The HybridSPE cartridge improved the removal efficiency of phospholipids, while 1 mL of methanol elution increased the extraction recoveries of targets. Fourteen UV-filters achieved good linearities, low detection limits (0.050 to 0.10 μg/L) and quantification limits (0.10 to 1.0 μg/L). Method accuracy and precision, extraction recoveries, and storage stabilities of all analytes met the criterion of 80–120 %. Moreover, this method was successfully applied for the determination of UV-filters in plasma randomly collected from adults. Nine of 14 UV-filters were determined and their concentrations were distributed widely, suggesting a big variation of individual UV-filters exposure.

Pharmacokinetic study of multicomponent in Hong-Hua-Xiao-Yao tablet.

Hong-Hua-Xiao-Yao tablet (HHXYT) is attracting attention increasingly because of its use in treatment of mammary gland hyperplasia (MGH) and menopausal syndrome. However, its pharmacokinetics remains unclear. This study developed a sensitive and rapid method for simultaneous determination of 10 compounds of HHXYT in rat plasma by liquid chromatography-tandem mass spectrometry and to compare the pharmacokinetics of these compounds in MGH rats and sham operated rats. The linearity, accuracy, precision, stability and matrix effect were within acceptable ranges. This established method was successfully applied to a pharmacokinetics study of 10 compounds in sham operated and MGH rats. According to the results, the bioavailability of glycyrrhetinic acid was highest in MGH rats and sham operated rats. The mean residence times of glycyrrhetinic acid and glycyrrhetinic acid 3-O-glucuronide were higher than those of the other compounds while the mean residence time and half-life of liquiritin, isoliquiritin and paeoniflorin were lower. Some pharmacokinetic parameters of ormononetin, liquiritigenin, isoliquiritigenin, liquiritin, isoliquiritin, paeoniflorin, protocatechuic acid and senkyunolide I were significantly different between MGH rats and sham operated rats. This study elucidated the dynamic changes of multiple components in rats after oral administration of HHXYT systematically and comprehensively, which provided guidance for clinical application.

Determination of the Carbamate Pesticides Fuberidazole and Pirimicarb in Crayfish (Procambarus Clarkii) Using Excitation-Emission Fluorescence Matrices with Self-Weighted Alternating Trilinear Decomposition (SWATLD)

Fuberidazole and pirimicarb are carbamate pesticides for insect control. There is pesticide accumulation through the food chain that may ultimately migrate into the human body through the crayfish. Here a rapid method for simultaneous determination of fuberidazole and pirimicarb in crayfish is reported. The excitation-emission fluorescence matrix was obtained by simple pretreatment of crayfish meat using acetonitrile, and qualitative and quantitative information was separated from overlapping spectra using the self-weighted alternating trilinear decomposition. The detection limits of the pesticides for fuberidazole and pirimicarb were 0.068 mg/kg and 0.160 mg/kg, respectively, and the limits of quantitation were 0.207 mg/kg and 0.485 mg/kg. The average recoveries were 90.79% and 98.77%. The results show that a combination of excitation-emission fluorescence matrix and alternating trilinear decomposition can be used for the determination of fuberidazole and pirimicarb in crayfish with simple pretreatment using acetonitrile.

A simple, rapid method for simultaneous determination of multiple elements in serum by using an ICP-MS equipped with collision cell

We developed an inductively coupled plasma mass spectrometry method for testing 23 elements, namely, Mg, Al, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Rb, Sr, Mo, Cd, Sn, Sb, Ba, W, Tl, Pb, and U, in human serum. The serum samples were analyzed after diluting 1/25 with 0.5% nitric acid, 0.02% Triton-X-100, and 2% methanol. Sc, In, Y, Tb, and Bi were assigned internal standards to correct the baseline drift and matrix interference. The kinetic energy discrimination mode of the instrument with helium gas as the collision gas eliminated polyatomic interference. All 23 elements exhibited excellent linearity in their testing range, with a coefficient of determination ≥ 0.9996. The limits of detection of the 23 elements were within the range of 0.0004–0.2232 µg/L. The intra- and inter-day precision (relative standard deviation) were < 12.19%. The recoveries of the spiked standard for all elements were 88.98–109.86%. Among the 23 elements of the serum reference materials, the measured results of Mg, Al, Cr, Mn, Fe, Co, Ni, Cu, Zn, and Se were within the specified range of the certificate, and the results of the other elements were also satisfactory. The developed method was simple, rapid, and effective, and only 60 μL sample was consumed. A total of 1000 serum samples from healthy individuals were randomly selected from the Henan Rural Cohort, which reflects the status of serum elements in rural adults from the Northern Henan province of central China.

Simultaneous Determination of Four Tetracycline Antibiotics Residues in Chicken by Solid Phase Extraction Coupled with High Performance Liquid Chromatography

Objective: To establish a simple and rapid method for simultaneous determination of Tetracycline, Oxytetracycline, Chlortetracycline and Doxycycline in chicken. Methods: After optimized sample pretreatment and chromatographic conditions, tetracycline antibiotics in spiked chicken were extracted by ultrasonic extraction with Na2EDTA-Mcllvaine buffer solution (pH=4.0), purified and enriched by HLB solid phase extraction column, separated by Shim-pack GIST C18 column (4.6&amp;times;150 mm, 3 &amp;mu;m), methanol-acetonitrile-oxalic acid (1:2:7, V: V: V) as the mobile phase, the flow rate was 0.9 mL/min, the UV detection wavelength was 350 nm, and the peak area was quantified by external standard method. Results: The linearity of the four tetracycline antibiotics was good in the range of 0.05-1 mg/kg (r＞0.997), and the detection limits were 2.53 &amp;mu;g/kg ~ 5.94 &amp;mu;g/kg according to the S/N ratio (S/N) of 3. The relative standard deviations (RSD, n=6) of precision were 1.51%-4.80%. The recoveries were from 76.81% to 96.34%. Conclusion: The method has good selectivity, high accuracy and reproducibility, and is suitable for simultaneous determination of four tetracycline antibiotics in chicken.

Hydrophilic Interaction Chromatography with Sulfobetaine Zwitterionic Polymer-Bonded Stationary Phases

A rapid method for simultaneous determination of two statin drugs based on zwitterionic chromatography (ZIC) had been developed and validated. The development method included examining the effects of chromatographic conditions, including the percentage of organic modifier, pH values, ionic strength of the acetate buffer, and the predominant retention mechanismand#39;s experimental determination. Separation developed by two zwitterionic stationary phases (100 mm and#215; 4.6 mm I.D., 3.5and#181;). The influence of various spacer lengths was being used as an examination tool on atorvastatin and rosuvastatin retention behaviours. Two zwitterionic stationary phases and a mobile phase consisting of acetonitrile and acetate (pH = 4.75, 40 mM) in a ratio of 80:20 V/V were used to achieve optimum chromatographic conditions. The methods had been validated for linearity, accuracy, and precision. This validation shows that the ZIC-HILIC methods proposed were sufficient for quantification analysis of atorvastatin and rosuvastatin. Quantifications were achieved with U.V. detection at 240 nm over the concentration range of 0.1–7.0 μg mL-1 for atorvastatin and rosuvastatin, respectively.

Potential value and chemical characterization of gut microbiota derived nitrogen containing metabolites in feces from Periplaneta americana (L.) at different growth stages

The American cockroach, Periplaneta americana (L.), is able to highly survive in various complicated environments around the globe, and often considered as a pest. In contrast, billions of P. americana have been massively reared in China and extensively used as a medicinal insect, due to its function for preventing and treating ulceration and heart failure. Considering the possibility that microbiota-derived metabolites could be an effective source to identify promising candidate drugs, we attempted to establish a rapid method for simultaneous determination of gut microbiota metabolites from medicinal insects. In this study, network pharmacology approach and ultra-performance liquid chromatography (UPLC) technique were employed to reveal the potential pharmacological activity and dynamics variation of nitrogen-containing metabolites (NCMs) originated from the gut microbiota of breeding P. americana at different growth stages. A metabolites-targets-diseases network showed that NCMs are likely to treat diseases such as ulceration and cancer. The analysis of NCMs' content with the growth pattern of P. americana indicated that the content of NCMs declined with P. americana aging. Both principal component analysis and orthogonal partial least squares discriminant analysis suggested that 8-hydroxy-2-quinolinecarboxylic acid and 8-hydroxy-3,4-dihydro-2(1H)-quinolinone are the potential differential metabolic markers for discriminating between nymphs and adults of P. americana. Moreover, the developed UPLC method showed an excellent linearity (R2 > 0.999), repeatability (RSD < 2.6%), intra- and inter-day precisions (RSD < 2.2%), and recovery (95.5%–99.0%). Collectively, the study provides a valuable strategy for analyzing gut microbiota metabolites from insects and demonstrates the prospects for discovering novel drug candidates from the feces of P. americana.

Rapid simultaneous determination of ketamine and midazolam in biological samples using ion mobility spectrometry combined by headspace solid-phase microextraction

Ketamine (Ket) and midazolam (Mdz) are among well-known anesthetic agents which frequently coadministered in surgical procedures and emergency department. Only a few reports have been published for the simultaneous analysis of these compounds. In the present study, we reported a simple, sensitive, and rapid method for simultaneous determination of Ket and Mdz based on headspace solid-phase microextraction coupled with ion mobility spectrometry (HS-SPME-IMS). Ion mobility spectrometer operated under positive mode of a corona discharge ionization source using ammonia as a dopant. The effective parameters on the extraction process consisting of pH of the sample, extraction temperature, extraction time, salt concentration were optimized. The calibration plots exhibited good linearity over the concentration ranges of 10-800 and 100-1500 µg L−1 and detection limit of 8.9 and 52 µg L−1 for Ket and Mdz respectively with correlation coefficients greater than 0.99. The relative standard deviation (RSD) for five replicate measurements was determined to be less than 8%. Finally, the applicability of the proposed method was tested in human plasma and serum samples. These tests showed that the matrix in serum samples interfere with midazolam determination but quantitative recoveries from 85 to 95 % were obtained for both drugs in the human plasma samples. The method herein provides simple and suitable approach while minimizing sample preparation and the overall complexity of the analysis in comparison to existing methodologies.

Rapid and simultaneous determination of trigonelline, caffeine, and chlorogenic acid in green coffee bean extract.

A simple, inexpensive, and rapid method for simultaneous determination of trigonelline, caffeine, and chlorogenic acid from green coffee bean extract was proposed based on salting‐out assisted liquid–liquid extraction, using QuEChERS salt and acetonitrile followed by UV‐Vis analysis. The proposed method represents acceptable linearity for trigonelline (0.9978), caffeine (0.9995), and chlorogenic acid (0.9996) with excellent correlation (0.93 and 0.83) for trigonelline and caffeine, respectively, when compared to RP‐HPLC‐DAD. The proposed method could be used in coffee industries for quality control and geographical origin traceability studies of green coffee samples.

A Reliable and Rapid Method for Simultaneous Determination of Furfural and Hydroxymethyl Furfural in Oil Refinery Wastewaters by Ant Colony/Partial Least-Squares Analysis

A Reliable and Rapid Method for Simultaneous Determination of Furfural and Hydroxymethyl Furfural in Oil Refinery Wastewaters by Ant Colony/Partial Least-Squares Analysis

Development and Validation of UPLC-MS/MS Method for Rapid Simultaneous Determination of Levothyroxine and Liothyronine in Human Serum

A simple ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS) method was developed and fully validated to simultaneously determine levothyroxine (LT4) and liothyronine (LT3) in human serum. Sample preparation was done through protein precipitation with acetonitrile. HyPURITY C18 column was selected to achieve rapid separation for LT4 and LT3 within 4 min. Electrospray ionization (ESI) under multiple reaction monitoring (MRM) was used to monitor the ion transitions for LT4 (m/z 777.54→731.52), LT3 (m/z 651.64→ 605.65) and internal standard LT4-D3 (m/z 780.53 →734.19), operating in the positive ion mode. The method was proved to be accurate (82.35% to 113.56%) and precise (0.73% to 8.28%) over concentration range of 50.37 ng/ml – 300.13 ng/ml for LT4 and 0.5 ng/ml – 50.37 ng/ml for LT3. The validated method could be applied for pharmacokinetic study or bioequivalence testing of combination products of LT4 and LT3.&#x0D; Keywords: Levothyroxine; Liothyronine; Ultra Performance Liquid Chromatographic; Mass Spectrometry; Human Serum

Simultaneous determination of 16 polycyclic aromatic hydrocarbons in source water and tap water by performance liquid chromatography with ultraviolet detector tandem fluorescence detector combined with solid phase extraction

To establish a rapid method for simultaneous determination of 16 polycyclic aromatic hydrocarbons(PAHs) in source water and tap water by performance liquid chromatography(HPLC) with ultraviolet detector(UV) tandem fluorescence detector(FLR). Source water was filtered by GF/C glass fiber filters and tap water were added ascorbic acid of 60 mg per liter to remove the residual chlorine when sampling. 500 mL water sample were sampled and adjusted pH 2 with phosphoric acid, then 10 mL methanol were added. Then samples were concentrated by styrene stilbene polymer solid phase extraction column, after loading samples, 50 percent methanol aqueous solution adjust pH 2 were used for washing bottle and the washed solution were continuum loaded. Then 80 percent methanol aqueous solution was used for removing impurity interference and elution with dichloromethane. The eluent was nitrogen blow to near dry after adding 100 μL 10 percent tween-20 methanol solutions(m/V). Acetonitrile was used for reconstitution, and then separated by PAH chromatography column using acetonitrile and pure water at gradient elution, and detected by UV tandem FLR detector. The linear ranges of 16 PAHs were 0. 5 to 500 ng/mL and the correlation coefficients were greater than 0. 999. The method detection limit and limits of quantification were 0. 3 to 5. 0 ng/L and 1. 2 to 20. 0 ng/L, respectively. The recoveries were in the range of 67. 2%-114. 1% with the relative standard deviations ranging from 1. 5%-14. 0%(n=6). Then the established method was used for the determination of 17 water samples, 8 kinds, 6 kinds and 7 kinds of PAHs were detected in source water, tap water and pipe net tap water, respectively. The method is rapid, sensitive and selective, and has been successfully applied for determination of 16 PAHs in source water and tap water.

Rapid and Simultaneous Measurement of Praeruptorin A, Praeruptorin B, Praeruptorin E, and Moisture Contents in Peucedani Radix Using Near-Infrared Spectroscopy and Chemometrics.

Peucedani Radix is a popular traditional Chinese medicine herb with a long history in China. Praeruptorin A (PA), praeruptorin B (PB), and praeruptorin E (PE) are usually taken as important quality indexes of Peucedani Radix. To establish a rapid method for simultaneous determination of PA, PB, PE, and moisture contents in Peucedani Radix using near-infrared (NIR) spectroscopy and chemometrics. One hundred twenty Peucedani Radix samples were analyzed with HPLC as a reference method. The NIR spectral scanning range was from 12000 cm-1 to 4000 cm-1. Partial least squares (PLS) regression algorithm was used to establish calibration models. Three variable selection methods were investigated, including variable importance in projection (VIP), competitive adaptive reweighted sampling (CARS), and Monte Carlo uninformative variable elimination (MCUVE). The performances of the established models were evaluated by root-mean-square error (RMSEC) and determination coefficient (Rc2) of calibration set, root-mean-square error (RMSEP) and determination coefficient (Rp2) of prediction set, and residual predictive deviation (RPD). A clear ranking of the performance of the calibration models could be as follows: CARS-PLS > MCUVE-PLS > VIP-PLS > Full-PLS. For CARS-PLS, Rp2, RMSEP, and RPD of the prediction set are as follows: 0.9204, 0.0860%, and 3.5850 for PA; 0.8011, 0.0431%, and 2.0868 for PB; 0.8043, 0.0367%, and 2.1569 for PE; and 0.9249, 0.3350%, and 3.6551 for moisture, respectively. The NIR spectroscopy combined with CARS-PLS calibration models could be used for rapid and accurate determination of PA, PB, PE, and moisture contents in Peucedani Radix samples.

A simple, cost-effective and rapid method for simultaneous determination of Strychnos nux-vomica alkaloids in blood and Ayurvedic medicines based on ultrasound-assisted dispersive liquid-liquid microextraction-thin-layer chromatography-image analysis.

A simple, rapid, cost-effective and green analytical method is developed based on ultrasound-assisted dispersive liquid-liquid microextraction (US-DLLME) coupled to thin-layer chromatography (TLC)-image analysis for the simultaneous determination of two major alkaloids of Strychnos nux-vomica L i.e., strychnine and brucine. The method is composed of three steps, namely (i) US-DLLME by injecting a mixture of 100-μL chloroform (extraction solvent) and 1-mL methanol (disperser solvent) in 5mL of aqueous sample, followed by ultrasonication and centrifugation, (ii) TLC of 20μL of sedimented phase with methanol: ammonia (100:1.5, v/v) as the mobile phase and visualization under ultraviolet radiation (254nm) and (iii) photography of TLC plate and quantification of spots by image analysis using freely available imageJ software (National Institute of Health, Bethesda, MD, USA). The limit of detection and limit of quantification for both alkaloids were found to be in the range of 0.12-0.15 and 0.36-0.48μg/spot, respectively. The method was found to be linear in the range of 0.5-5μg/spot with correlation coefficient (R2) of 0.995 and 0.997 for strychnine and brucine, respectively. The developed method was successfully applied for the determination of strychnine and brucine in Ayurvedic formulations and blood samples. The method does not require any sophisticated instrument and handling skills and can be adopted for rapid analysis of strychnine and brucine in forensic toxicological laboratories.

A rapid method for simultaneous determination of nitrate, nitrite and thiocyanate in milk by CZE-UV using quaternary ammonium chitosan as electroosmotic flow inverter

This paper proposes a rapid method for the simultaneous determination of nitrate, nitrite and thiocyanate in different milk samples (cow, goat and soy) using capillary zone electrophoresis. The separations were conducted in a fused silica capillary dynamically coated with quaternary ammonium chitosan, with a total length of 48.5 cm (40 cm effective x 75 μm internal diameter) and direct detection in the UV region at 210 nm. The background electrolyte (BGE) was composed of 30 mmol L−1 of aminocaproic acid and 24 mmol L1 of perchloric acid (pH 3.85).A typical anodic electroosmotic flow of -31 × 10-9 m2 V−1 s−1 was observed at the pH of the separations. Bromate was used as the internal standard. The samples were injected by hydrodynamic pressure (50 mbar, 40 s) and the separation voltage was −30 kV. The proposed method was validated and presented good linearity (R2> 0.99) in the linear range of 0.1–4.0 mg L−1. The ranges of the limit of detection (LOD) and limit of quantification (LOQ) were 0.03-0.04 and 0.05–0.07 mg L−1, respectively. The intra-day and inter-day precision values were better than 4.2 and 8.7 %, respectively. Recovery values ranged from 85 to 104% for the different samples of milk. The proposed method was applied in 12 commercial samples with run times of less than 2 min. The good analytical performance indicates that the method proposed is a promising alternative for the determination of nitrate, thiocyanate and nitrite in milk samples.

Simultaneous Determination of Various Phosphates in Water-Soluble Ammonium Polyphosphate

Based on ion chromatography, this study developed a rapid method for simultaneous determination of linear polyphosphates (PPs) of orthophosphate (P1), pyrophosphate (P2), trimetaphosphate (P3m), tripolyphosphate (P3), tetraphosphate (P4), pentaphosphate (P5), and hexaphosphate (P6) in water-soluble ammonium polyphosphate (WAPP). Investigation indicated that the retention of PPs in column was endothermic and cooling column benefited the elution of PPs. With adjusting the elution mode, eluent (KOH) concentration, gradient time, flowrate, and column temperature, the optimized results were as follows: the injection volume of sample was 1.3 μL, column temperature was 30 °C, and flowrate of the eluent was 1.2 ml min−1. The linear equations for six phosphates are: y = 0.011cP1 + 0.021 (r = 0.9998), y = 0.012cP2 + 0.023, y = 0.011cP3m − 0.013 (r = 0.9997), y = 0.12cP3 + 0.017 (r = 0.9999), y = 0.011cP4 + 0.004 (r = 0.9983), y = 0.011cP5 − 0.082 (r = 0.9962), and y = 0.013cP6 − 0.029 (r = 0.9989), respectively. The determination ranges are: 1–500 mg L−1 for P1, P2, P3m, and P3; and 1–100 mg L−1 for P4, P5, and P6. The recovery is in the range 95–104% for P1, P2, P3m, P3, P4, P5, and P6; the detection limit is in the range 0.17–0.54 mg L−1 and RSDs of intra- and inter-day determination are 0.56–2.51% (n = 5) for seven PPs, and the analysis period is 15 min. The method was consistent with both gravimetric method and molybdenum blue method, while the RSD was in the range 0.61–1.87%. This rapid method can be applied in the determination of total phosphorus and various phosphates in PPs.

Development a simple and rapid HPLC-ESI-Q-TOF/MS method for determination of short- and medium- chain chlorinated paraffins in human serum

This study established a simple and rapid method for simultaneous determination of short-chain chlorinated paraffins (SCCPs) and medium-chain chlorinated paraffins (MCCPs) in human serum by high performance liquid chromatography coupled with electron spray ionization quadrupole time-of-flight mass spectrometry (HPLC-ESI-Q-TOF/MS). A simple pretreatment procedure of protein precipitation by acetonitrile coupled with liquid-liquid extraction by n-hexane was employed for extraction and purification. The purified samples were separated by a PFP chromatographic column. This method could effectively eliminate the matrix effect by lipids and other matrix substances in serum samples with less time and solvent consuming. 76 congener groups of SCCPs and MCCPs with C10-C17 and Cl5-Cl13 were quantified by their [M-H]− ions. Method detection limit (MDL) were 1.0–8.0 ng mL−1 for ∑SCCPs and ∑MCCPs. Recoveries were 98.4 ± 4.42%, 98.8 ± 3.96% and 90.7 ± 2.79% for SCCPs and 93.1 ± 6.67%, 108 ± 1.21% and 90.8 ± 3.78% for MCCPs at spiking concentrations of 20, 50 and 200 ng·mL−1, respectively. The relative standard deviations (RSDs) of intra- and inter-day variations were 1.41% and 9.84% for SCCPs, and 4.23% and 6.26% for MCCPs. The suitability of the developed method was demonstrated through the application to analysis of SCCPs and MCCPs in human serum samples.

Simultaneous determination of synthetic edible pigments in beverages by titania-based RP-HPLC

A rapid method for simultaneous determination of five synthetic edible pigments (SEPs) including tartrazine (TA), ponceau 4R (PO), sunset yellow (SY), brilliant blue (BB) and erythrosine (ER) in beverages with titania-based RP-HPLC has been developed. The good linear relationships were obtained in the concentration ranges of 2.5–40 μg mL−1 for TA, PO and SY, 0.75–12 μg mL−1 for BB, and 1.25–20 μg mL−1 for ER, respectively. The detection limits (LODs) of five SEPs were 0.042, 0.021, 0.042, 0.0005, and 0.021 μg mL−1, respectively. The average recoveries were between 92.2% and 106.3%. Relative standard deviations (RSD, n = 7) for five SEPs were less than 1.18%. The precision and accuracy of the method can meet the requirements of HPLC analysis. In addition, the thermodynamic parameters of retention of the pigments in the titania column such as enthalpy (ΔHο), entropy (ΔSο) and Gibbs free energy (ΔGο) were also determined.

Simultaneous determination of pesticides and mycotoxins in wine by direct injection and liquid chromatography-tandem mass spectrometry analysis

A simple and rapid method for simultaneous determination of pesticides and mycotoxins in red wine is presented. Sample preparation approach, called direct injection, consists of a sequence of only three steps: centrifugation, dilution and filtration. The analysis of extracts were performed by UPLC-MS/MS for determination of pesticides and mycotoxins. The method was assessed for linearity, limits of detection and quantification, matrix effects, selectivity, accuracy and precision. For recovery experiments, mycotoxins were divided in two groups according to their sensitivity in the UPLC-MS/MS system. More than 80% of the mycotoxins were reliably quantified at the lowest spike level studied (1 μg kg−1 for group 1 and 50 μg kg−1 for group 2). From the 185 evaluated pesticides, 144 showed acceptable results at 10 μg kg−1, the lowest spiked level. Matrix effects were, in most of the cases, negative, and that was observed for both pesticides and mycotoxins.