Ultra-fast Liquid Chromatography-tandem Quadrupole Mass Research Articles

Extraction Optimization of Six Alkaloids and Four Lignans in Zanthoxylum armatum by Orthogonal Design and Ultra-fast Liquid Chromatography–tandem Quadrupole Mass Spectrometry

Alkaloids and lignans in Zanthoxylum armatum display important biological activities, but the quanitification method of alkaloids has not been reported. In this study, an effective extraction method was developed through an orthogonal design, and ten compounds in roots, stems, branches and leaves of Zanthoxylum armatum were simultaneously quantified by ultra-fast liquid chromatography–tandem quadrupole mass spectrometry (UFLC–MS/MS). The roots, stems, branches and leaves of Z. armatum were ultrasonically extracted with methanol (solvent–to–sample ratio 100 : 1, v/w) for 10 min. An UFLC–MS/MS method was developed with a gradient UFLC mobile phase and triple quadruple tandem mass spectrometry with electrospray ionization in the positive ion mode. The method was validated for linearity, precision, repeatability and accuracy. The limits of detection and quantification were within 0.01–7.5 and 0.04–30 ng/mL, respectively. The root samples collected from Tian’e County were abundant in N-methylanhydrotetrahydroberberrubine A, escholidine perchlorate and pinoresinol monomethyl ether, eudesminthe.

Fast throughput determination of 21 allergenic disperse dyes from river water using reusable three-dimensional interconnected magnetic chemically modified graphene oxide followed by liquid chromatography–tandem quadrupole mass spectrometry

We report the template-free fabrication of three-dimensional hierarchical nanostructures, i.e., three-dimensional interconnected magnetic chemically modified graphene oxide (3D-Mag-CMGO), through a simple and low-cost self-assembly process using one-pot reaction based on solvothermal method. The excellent properties of the 3D-Mag-CMGO are characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), vibrating sample magnetometer (VSM), FTIR, elementary analyzer (EA) and X-ray photoelectron spectroscopy (XPS). The easiness-to-handle of the magnetic dispersive solid phase extraction (Mag-dSPE) procedure is developed for preconcentration of 21 allergenic disperse dyes from river water. The obtained results show the higher extraction capacity of 3D-Mag-CMGO with recoveries between 80.0–112.0%. Furthermore, an ultra-fast liquid chromatography-tandem quadrupole mass spectrometry (UFLC–MS/MS) method for determination of 21 allergenic disperse dyes in river at sub-ppt levels has been developed with pretreatment of the samples by Mag-dSPE. The limits of quantification (LOQs) for the allergenic disperse dyes are between 0.57–34.05ng/L. Validation results on linearity, specificity, trueness and precision, as well as on application to the analysis of 21 allergenic disperse dyes in fifty real samples demonstrate the applicability to environment monitoring analysis.

PRiME pass-through cleanup for the fast determination of aflatoxins in human serum by using LC-MS/MS

A novel, simple and sensitive method based on the use of a PRiME (process, robustness, improvements, matrix effects, ease of use) pass-through cleanup procedure combined with ultra-fast liquid chromatography-tandem quadrupole mass spectrometry (UFLC-MS/MS) for the determination of 4 AFs, i.e., AFB1, AFB2, AFG1 and AFG2 in human serum, was developed and validated. The effective PRiME pass-through cleanup procedure using the Oasis PRiME HLB cartridge was optimized for the extraction of AFB1, AFB2, AFG1 and AFG2 in human serum. The obtained results demonstrated the higher extraction capacity of the PRiME pass-through cleanup procedure with recoveries between 92.1% and 102%. The limits of detection (LODs) for AFB1, AFB2, AFG1 and AFG2 were 0.048 μg L−1, 0.069 μg L−1, 0.043 μg L−1 and 0.14 μg L−1, respectively. Validation results on linearity, specificity, accuracy and precision, as well as on application to the analysis of AFs in 10 liver cancer volunteers demonstrated the applicability to clinical studies.

Fast determination of catecholamines in human plasma using carboxyl-functionalized magnetic-carbon nanotube molecularly imprinted polymer followed by liquid chromatography-tandem quadrupole mass spectrometry

A novel, simple and sensitive method based on the use of dispersive micro-solid-phase extraction (d-μ-SPE) procedure combined with ultra-fast liquid chromatography–tandem quadrupole mass spectrometry (UFLC–MS/MS) for the determination of catecholamines, i.e., dopamine (DA), norepinephrine(NE) and epinephrine (E), was developed and validated. The novel catecholamines molecularly imprinted polymer (MIP) on the surface of carboxyl-functionalized magnetic-carbon nanotube (CF@m-CNTs-MIP) was synthesized and characterized by vibrating sample magnetometer (VSM), scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). The CF@m-CNTs-MIP was used as the d-μ-SPE sorbent to extract catecholamines from human plasma samples. The obtained results demonstrated the higher extraction capacity of CF@m-CNTs-MIP with recoveries between 87.5–110%. The limits of quantification (LOQs) for NE, E and DA were 76ng/L, 18ng/L and 10ng/L, respectively. Validation results on linearity, specificity, accuracy, precision and stability, as well as on application to the analysis of catecholamines in 120 healthy volunteers demonstrated the applicability to clinical studies.

Fast determination of 24 steroid hormones in river water using magnetic dispersive solid phase extraction followed by liquid chromatography-tandem mass spectrometry.

The easiness-to-handle of the magnetic dispersive solid phase extraction (Mag-dSPE) procedure was developed for preconcentration of 24 steroid hormones in river water. Ethylenediamine-functionalized magnetic carbon nanotubes (EDA@Mag-CNTs) were synthesised by a simple one-pot reaction and were used as sorbent in Mag-dSPE procedure. The properties of the EDA@Mag-CNTs were characterized by transmission electron microscopy (TEM) and vibrating sample magnetometer (VSM). An ultra-fast liquid chromatography-tandem quadrupole mass spectrometry (UFLC-MS/MS) method for determination of 24 steroid hormones in river water at nanograms per liter had been developed with pretreatment of the samples by Mag-dSPE. The obtained results demonstrated the higher extraction capacity of EDA@Mag-CNT Mag-dSPE with recoveries between 82.1 and 113%. The limits of quantification (LOQs) for the steroid hormone were between 0.020 and 1.00 ng/L. The developed method had been successfully applied to 60 river water samples, and it was confirmed that EDA@Mag-CNT Mag-dSPE was a highly effective extraction method for the steroid hormone analyses.

Rapid method for quantification of seven synthetic pigments in colored Chinese steamed buns using UFLC-MS/MS without SPE.

Synthetic pigments are still used instead of natural pigments in many foods and their residues in food could be an important risk to human health. A simple and rapid analytical method combining the low-cost extraction protocol with ultra-fast liquid chromatography-tandem quadrupole mass spectrometry (UFLC-MS/MS) was developed for the simultaneous determination of seven synthetic pigments used in colored Chinese steamed buns. For the first time, ethanol/ammonia solution/water (7:2:1, v/v/v) was used as extraction solution for the synthetic pigments in colored Chinese steamed buns. The results showed that the property of the extraction solution used in this method was more effective than critic acid solution, which is used in the polyamide adsorption method. The limits of quantification for the seven synthetic pigments ranged from 0.15 to 0.50 μg/kg. The present method was successfully applied to samples of colored Chinese steamed buns for food-safety risk monitoring in Zhejiang Province, China. The results found sunset yellow pigment in six out of 300 colored Chinese steamed buns (from 0.50 to 32.6 μg/kg).

Rapid determination of memantine in human plasma by using nanoring carboxyl-functionalized paramagnetic molecularly imprinted polymer d-μ-SPE and UFLC-MS/MS.

A novel, simple, and sensitive method based on the use of dispersive micro-solid-phase extraction (d-μ-SPE) procedure combined with ultra-fast liquid chromatography-tandem quadrupole mass spectrometry (UFLC-MS/MS) for the determination of memantine (ME) was developed and validated over the linearity range 0.05-10.0 µg/L with 100 μL of human plasma using memantine-D6 (ME-D6) as the internal standard. The novel nanoring carboxyl-functionalized paramagnetic molecularly imprinted polymer (NR-CF-Mag-MIP) was synthesized by ultrasound-assisted suspension polymerization, using ME as a template molecule, methacrylic acid as a functional monomer, and divinylbenzene as a cross-linking agent. The NR-CF-Mag-MIP was used as the d-μ-SPE sorbent to extract ME from human plasma samples. The obtained results demonstrated the higher extraction capacity of NR-CF-Mag-MIP with recoveries between 97.6 and 101%. The limits of quantification (LOQs) for ME was 0.015 µg/L. Validation results on linearity, specificity, accuracy, precision, and stability, as well as on application to the analysis of samples taken up to 480 h after oral administration of 20 mg (two 10 mg capsules) of ME in healthy volunteers demonstrated the applicability to bioequivalence studies.

Rapid determination of trace dicyandiamide in mussels from Zhejiang coast by ultra-fast liquid chromatography-tandem mass spectrometry with isotope internal standard dilution technique.

In this study, a rapid and accurate ultra-fast liquid chromatography-tandem quadrupole mass spectrometry (UFLC-MS/MS) method coupled with the isotope internal standard dilution technique was established and validated to determine trace dicyandiamide (DCD) in mussels. The sample was extracted by acetonitrile, and chromatographic separations were performed on an Acquity UPLC BEH Amide column by using water-acetonitrile (9:91, v/v) as the mobile phase within 3 min. DCD was determined by using DCD-(15)N4 as an internal standard. The results showed that the recoveries were between 96.2 and 103 % with relative standard deviations (RSDs) in the range of 0.6-6.0 %. The limit of quantification (LOQ) was 0.05 μg/kg. This method can be applied to the routine analysis for the rapid and sensitive determination of trace DCD in mussels. Overall, the data reiterate the importance of investigating the presence of DCD in marine biological samples, which can act as food quality controls for human health.

Fast determination of seven synthetic pigments from wine and soft drinks using magnetic dispersive solid-phase extraction followed by liquid chromatography–tandem mass spectrometry

A novel, simple and sensitive method based on the use of magnetic dispersive solid-phase extraction (M-dSPE) procedure combined with ultra-fast liquid chromatography-tandem quadrupole mass spectrometry (UFLC–MS/MS) was developed to determine seven synthetic pigments (tartrazine, amaranth, carmine, sunset yellow, allura red, brilliant blue and erythrosine) in wines and soft drinks. An amino-functionalized low degrees of cross-linking magnetic polymer (NH2-LDC-MP) was synthesized via suspension polymerization, and characterized by transmission electron microscopy (TEM). The NH2-LDC-MP was used as the M-dSPE sorbent to remove the matrix from the solution, and the main factors affecting the extraction were investigated in detail. The obtained results demonstrated the higher extraction capacity of NH2-LDC-MP with recoveries between 84.0 and 116.2%. The limits of quantification (LOQs) for the seven synthetic pigments were between 1.51 and 5.0μg/L in wines and soft drinks. The developed M-dSPE UFLC–MS/MS method had been successfully applied to the real wines and soft drinks for food-safety risk monitoring in Zhejiang Province, China. The results showed that sunset yellow was in three out of thirty soft drink samples (2.95–42.6μg/L), and erythrosine in one out of fifteen dry red wine samples (3.22μg/L), respectively. It was confirmed that the NH2-LDC-MP was a kind of highly effective M-dSPE materials for the pigments analyses.

Fast determination of 22 sulfonamides from chicken breast muscle using core–shell nanoring amino-functionalized superparamagnetic molecularly imprinted polymer followed by liquid chromatography-tandem mass spectrometry

A novel, simple and sensitive method was developed for the simultaneous determination of 22 sulfonamides (SAs) in chicken breast muscle by using the dispersive micro-solid-phase extraction (d-μ-SPE) procedure combined with ultra-fast liquid chromatography-tandem quadrupole mass spectrometry (UFLC-MS/MS). The excellent core–shell nanoring amino-functionalized superparamagnetic molecularly imprinted polymer (CS-NR-Mag-MIP) was used as sorbent, and the main factors affecting the extraction efficiency were investigated in detail. All target compounds showed good linearities in the tested range with correlation coefficients (r) higher than 0.9980. The mean recoveries were in the range of 85.0–112.2% at low, medium and high concentration levels (0.1, 1.0 and 5.0ng/g). The intra-day and inter-day relative standard deviations (RSDs) were lower than 6.0% and 8.9%, respectively. The limits of quantification for the 22 SAs were between 0.013 and 0.099ng/g. The developed d-μ-SPE-UFLC-MS/MS method had been successfully applied to the chicken breast muscle samples for food-safety risk monitoring in Zhejiang Province, China. The results showed sulfamethazine, sulfamethoxazole and sulfaquinoxaline in five out of three hundred collected samples were detected with concentrations of 0.418–2.28, 16.4 and 2.93ng/g, respectively. It was confirmed that the CS-NR-Mag-MIP was a kind of highly effective d-μ-SPE materials used for the SAs analyses.

Application of nanoring amino-functionalized magnetic polymer dispersive micro-solid-phase extraction and ultra fast liquid chromatography–tandem mass spectrometry in dicyandiamide residue analysis of powdered milk

In this study, a rapid and accurate ultra-fast liquid chromatography-tandem quadrupole mass spectrometry (UFLC-MS/MS) method combined with dispersive micro-solid-phase extraction (d-µ-SPE) using a core-shell nanoring amino-functionalized magnetic polymer (CS-NR-MP) was established and validated to determine trace dicyandiamide (DCD) in powdered milk. The developed d-µ-SPE cleanup procedure can dramatically reduce the matrix in samples, and lead to a significant reduction in absolute matrix effects. Chromatographic separation was performed on an Acquity UPLC BEH Amide column by using water-acetonitrile (9:91, v/v) as the mobile phase within 2 min. DCD was quantitatively analyzed by using DCD-(15)N2(13)C2 as an internal standard. The results showed that the recoveries were between 99.8 and 105.6% with RSDs in the range of 0.5-4.9%. The target compound had good linearity in the range of 0.1-20.0 µg L(-1) with a correlation coefficient (r) of 0.9996. The limit of quantification (LOQ) was 0.06 µg kg(-1). This method can be used for the rapid and sensitive determination of ultratrace DCD residue in powdered milk samples.

Simultaneous analysis of eight phenolic environmental estrogens in blood using dispersive micro-solid-phase extraction combined with ultra fast liquid chromatography–tandem mass spectrometry

A novel, simple and sensitive method was developed for the simultaneous determination of eight phenolic environmental estrogens in blood by using the dispersive micro-solid-phase extraction (d-µ-SPE) procedure combined with ultra-fast liquid chromatography–tandem quadrupole mass spectrometry (UFLC–MS/MS). The excellent nanomaterials tetraethylenepentamine-functionalized magnetic polymer was used as an adsorbent, and the main factors affecting the extraction efficiency were investigated in detail. All target compounds showed good linearities in the tested range with correlation coefficients (r) higher than 0.999. The mean recoveries were in the range of 85.0–105.0%. The intra-day and inter-day relative standard deviations (RSDs) were lower than 4.9% and 5.2%, respectively. The limits of quantification for the eight phenolic environmental estrogens were between 0.075 and 0.42µgL−1. The developed method can be applied to the routine analyses for the determination of the eight phenolic environmental estrogens in blood samples.

Application of dispersive solid-phase extraction and ultra-fast liquid chromatography–tandem quadrupole mass spectrometry in food additive residue analysis of red wine

A novel and effective dispersive solid-phase extraction (dSPE) procedure with rapid magnetic separation using ethylenediamine-functionalized magnetic polymer as an adsorbent was developed. The new procedure had excellent clean-up ability for the selective removal of the matrix in red wine. An accurate, simple, and rapid analytical method using ultra-fast liquid chromatography–tandem quadrupole mass spectrometry (UFLC–MS/MS) for the simultaneous determination of nine food additives (i.e., acesulfame, saccharin, sodium cyclamate, aspartame, benzoic acid, sorbic acid, stevioside, dehydroacetic acid, and neotame) in red wine was also used and validated. Recoveries ranging from 78.5% to 99.2% with relative standard deviations ranging from 0.46% to 6.3% were obtained using the new method. All target compounds showed good linearities in the tested range with correlation coefficients (r) higher than 0.9993. The limits of quantification for the nine food additives were between 0.10μg/L and 50.0μg/L. The proposed dSPE–UFLC–MS/MS method was successfully applied in the food-safety risk monitoring of real red wine in Zhejiang Province, China.