This paper presents a new analytical method for the determination of morpholine residues in citrus and apples using a novel dispersive micro-solid-phase extraction (DMSPE), followed by ultrahigh-performance liquid chromatography-high-resolution mass spectrometry (UHPLC-HRMS). Samples were extracted with 1% formic acid in acetonitrile/water (1:1, v/v) and then cleaned up using the DMSPE procedure. Morpholine from the extract was adsorbed to a polymer cation exchange sorbent and eluted with ammonium hydroxide/acetonitrile (3:97, v/v) through a 1 mL syringe with a 0.22 μm nylon syringe filter. All of the samples were analyzed by UHPLC-HRMS/MS on a Waters Acquity BEH hydrophilic interaction chromatography column using 0.1% formic acid and 4 mM ammonium formate in water/acetonitrile as the mobile phase with gradient elution. The method showed good linearity (R(2) > 0.999) in the range of 1-100 μg/L for the analyte. The limit of detection and limit of quantitation values of morpholine were 2 and 5 μg/kg, respectively. The average recoveries of morpholine from the citrus and apple samples spiked at three different concentrations (5, 20, and 100 μg/kg) were in a range from 78.4 to 102.7%.
One hundred and one tea samples including green tea, dark tea, scented tea, black tea, and oolong tea were screened and confirmed for the contamination of 31 organochlorine pesticides (OCPs) and 19 pyrethroids (PYs) by gas chromatography-negative chemical ionization-mass spectrometry (GC-NCI-MS) and gas chromatography-tandem mass spectrometry (GC-MS/MS). 50 pesticides, 3 deuterium-labeled PYs, and 24 (13)C-labeled OCPs were separated well with the limits of detection (LODs) ranging from 0.02 to 4.5 μg/kg for GC-NCI-MS, and the positive samples were verified by GC-MS/MS with LODs of 0.1-5.0 μg/kg. High detection rates for some PYs, such as 63.4% for bifenthrin (not detected (ND)-3.848 mg/kg), 55.4% for λ-cyhalothrin (ND-3.244 mg/kg), 46.5% for cypermethrin (ND-0.499 mg/kg), and 24.8% for fenvalerate (ND-0.217 mg/kg), were found in the 101 tea samples. Endosulfan, DDTs, HCHs, and heptachlor, the persistent OCPs, were frequently detected with rates of 63.4% (ND-1.802 mg/kg), 56.4% (ND-0.411 mg/kg), 24.8% (ND-0.377 mg/kg), and 15.8% (ND-0.100 mg/kg), respectively.
A liquid chromatography-linear ion-trap spectrometry (LC-MS³) method using β-receptor molecular-imprinted polymer (MIP) solid-phase extraction (SPE) as clean-up was developed to determine simultaneously and confirmatively residues of 25 β₂-agonists and 21 β-blockers in urine samples. Urine samples were subjected to enzymatic hydrolysis by β-glucoronidase/arylsulphatase, and then extracted with perchloric acid. Sample clean-up was performed using β-receptor MIP SPE. A Supelco Ascentis® express Rp-Amide column was used to separate the analytes, and MS³ detection used an electrospray ionisation source in positive-ion mode. Recovery studies were carried out using blank urine samples fortified with the 46 analytes at the levels of 0.5, 1.0 and 2.0 μg l⁻¹. Recoveries were obtained ranging from 60.1% to 109.9% with relative standard deviations (RSDs, n = 7) from 0.5% to 19.4%. The limits of detection (LODs) and limits of quantitation (LOQs) of the 46 analytes in urine were 0.02-0.18 and 0.05-0.60 μg l⁻¹, respectively. As a result of the selective clean-up by MIP SPE and MS³ detection of the target drugs, the sensitivity and accuracy of the present method was high enough for monitoring β₂-agonist and β-blocker residues in urine samples. Satisfactory results were obtained in the process of the determination of positive urine samples.
Phthalate esters are environmental hormones present in food due to their migration from packaging materials and other polymers. Gas chromatography and liquid chromatography coupled with mass spectrometry are the most widely used techniques for trace phthalate ester determination. However, a major problem in the analysis is contamination during the sample pretreatment, resulting in false-positive results or over-estimated concentrations. In this study, a simple, rapid, and sensitive method for the determination of seventeen phthalate esters in liquor using high resolution mass spectrometry was developed. Samples were directly analyzed without pretreatment, which reduced contamination and improved the accuracy of the results. In addition, the total time required for the analysis of one sample was only 15 minutes. The method showed good linearity (R 2 > 0.995) in the ranges of 1 to 100 µg/L and 100 to 500 µg/L. The limits of detection and quantification were between 0.1 and 1.0 µg/L and 0.4 and 2.0 µg/L, respectively. The precision was evaluated by intra-day and inter-day measurements and expressed as the relative standard deviation (RSD). The values were less than 4.32% and 7.43%, respectively. The recovery values of phthalate esters from liquor fortified at 10, 50, 100, and 200 µg/L were determined to be 88.7% to 119.2%, with relative standard deviations of 0.3% to 9.6% (n ¼ 6). The method was suitable for the rapid screening and confirmation of phthalate esters in liquor.
A method for the simultaneous determination of 18 pesticide residues in red wine was developed using ultra high performance liquid chromatography-high resolution mass spectrometry (UPLC-HRMS) with isotope dilution technique. The red wine samples were extracted with acetonitrile, and the extracts were cleaned up with dispersive solid phase extraction (dSPE) using the mixture of N-propyl ethylene diamine (PSA) and C18 powder as sorbent. The extracted components were separated on a BEH C18 column by gradient elution. The qualitative and quantitative analyses were operated under full scan/data dependent MS/MS (ddms2) and targeted selective ion monitoring (tSIM) by high resolution mass spectrometry, respectively. Carbendazim-D4, chlorpyrifos-D10, imidacloprid-D4, methoxyfenozide-D9, pyrimethanil-D5 and tebuconazole-D6 were used as the internal standards to reduce the matrix effects. The response of each pesticide showed a good linearity in the range of 0.5-50 microg/kg with the correlation coefficient more than 0.999. The limits of detection and quantification for the 18 pesticides in the spiked blank red wine were 0.5 microg/kg and 1.0 microg/kg, respectively. The recovery results with spiked blank red wine samples at the levels of 1 to 40 microg/kg were satisfactory with average recoveries of 85.4% - 117.9% and the RSDs of 0.5%-6.1%. The method was applied for the determination of the red wine real samples from the market. Carbendazim, imidacloprid, pyrimethanil, tebuconazole and triadimenol were detected in the samples. The results show that the method is suitable for the rapid screening and quantitative analysis of pesticide residues in red wine.
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