About seller
An examination of the relative merits of acetonitrile precipitation and accelerated solvent extraction, two pretreatment methods, was conducted. Beyond this, the impact of various extraction conditions—including extraction time, extraction temperature, and the repetition of cycles—was scrutinized. Criteria for the optimal chromatographic conditions, including the column, temperature, and elution method, were identified. The complementary investigation into mass spectrometry conditions, such as collision energy and declustering potential of the target compound ion pairs, was subsequently performed. Reliable data were gathered using the best pretreatment methods and detection parameters, as determined through experimental results. Deionized water, acting as the extraction solvent, was used to process blood and urine samples via an accelerated solvent extractor. Centrifugal ultrafiltration, followed by 0.22 μm membrane filtration, was used to collect the supernatant, which was then diluted 50-fold prior to injection onto the chromatographic column for analysis. The eluent, a 150 mmol/L KOH solution, was used for the isocratic elution procedure on an Ion Pac AS20 IC column. The effluent, having been passed through a suppressor, was then introduced into a triple quadrupole mass spectrometer that executed MS/MS (ESI-) in multiple reaction monitoring (MRM) mode. The determined m/z value for the ion was within the range of 570 to 770, when the collisional energy (CE) was -150 eV and the dynamic prefilter (DP) was set to -200 volts. Quantitative analysis was conducted by applying an externally standardized method. The results indicated a substantial linear relationship for fluoroacetic acid, spanning concentrations from 0.5 to 5000 g/L (correlation coefficient r > 0.999). The limits of detection and quantification (LOD and LOQ) were found to be 0.014 g/L and 0.047 g/L, respectively. Fluoroacetic acid recovery rates in blood and urine were respectively 934%-958% and 962%-984%. The intra-day relative standard deviations (RSDs) for blood and urine samples were 8%–16% and 2%–10%, respectively. The inter-day RSDs, however, were significantly higher, ranging from 23%–38% for blood and 39%–69% for urine. Further investigation showed the matrix effects of this technique to be relatively weak, exhibiting -74% and -30% reduction in blood and urine samples, respectively. The established technique was applied to detect fluoroacetic acid in human blood and urine from a suspected poisoning, providing critical information that dramatically accelerated the resolution of the case. bcr-abl signal In terms of efficiency, the method significantly exceeded the performance of conventional detection methods. In essence, the method developed manifests high sensitivity and good repeatability, and is therefore appropriate for the rapid determination of fluoroacetic acid in human blood and urine. In addition, the method's independence from derivatization procedures ensures both simplicity and efficiency.Emerging chlorinated disinfection byproducts (DBPs), halobenzoquinones (HBQs), are increasingly prevalent in treated tap water and other water sources, such as entrainment water. Disinfection by-products, including trihalomethanes and haloacetic acids, are regulated, yet the compounds generated during water treatment with chlorine, chloramine, and chlorine dioxide, display more adverse effects. HBQs, posing a threat as potential bladder carcinogens, impact the nervous system negatively. Not only that, but they also induce genotoxic effects, resulting in the oxidative damage of DNA and proteins. It is anticipated that the risk of HBQs in aquatic products will escalate in light of the substantial increase in disinfection procedures for public facilities during the recent years. Consequently, the design and implementation of a method for accurately and sensitively identifying HBQs in aquatically-sourced products are imperative. For the purpose of determining and measuring HBQs in water samples, several analytical techniques are available, including gas chromatography, gas chromatography coupled with mass spectrometry, electrochemical procedures, liquid chromatography, and liquid chromatography combined with tandem mass spectrometry. No documented reports on the determination of HBQ levels in aquatic products have been found, as far as we know. Consequently, pretreatment is critical to the determination of HBQ, stemming from the intricate matrix effects of aquatic product samples. A sensitive and accurate method for the simultaneous determination of five HBQs in aquatic products was developed using the QuEChERS technique coupled with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). To optimize the QuEChERS procedure, a systematic investigation into the pretreatment conditions, including the extraction solvent and adsorbent, was undertaken. A 10 mL extraction solvent, comprising 10% methanol in acetonitrile and 0.1% formic acid, was used to extract the sample, which was subsequently dehydrated and centrifuged, incorporating sodium chloride and anhydrous magnesium sulfate. Purification of the supernatant was achieved using a QuEChERS packing material, which contained 50 mg N-propylethylenediamine (PSA), 30 mg graphitized carbon black (GCB), and 30 mg neutral alumina (Al2O3). The material was dried with nitrogen and concentrated. Employing a Waters ACQUITY UPLC BEH C18 column (100 mm × 2.1 mm, 1.7 µm) with a gradient elution procedure and 0.25% acetonitrile formate solution and 0.25% aqueous formic acid solution as the mobile phase, five HBQs were successfully separated. Final detection was performed using UPLC-MS/MS with negative electrospray ionization (ESI-) in multiple reaction monitoring (MRM) mode. A matrix-matched external standard method was employed for quantitative analysis. The proposed method facilitated the swift separation of the five HBQs in 6 minutes, reflecting a much shorter separation time compared to previous investigations. By generating a matrix-matched calibration curve, the matrix effect was ascertained. Observations indicated that 25-dichloro-14-benzoquinone (25-DCBQ) acted to increase matrix levels, whereas the other HBQs demonstrated a tendency to reduce matrix levels. Among the compounds tested, tetrachlorobenzoquinone (TCBQ) showed potent inhibitory effects. In optimally configured laboratory settings, the five HBQs exhibited a strong, linear correlation within a concentration range of 10 to 500 grams per liter, as evidenced by correlation coefficients (r) exceeding 0.9992. Detection limits for the method spanned a range of 0.015 to 0.008 grams per kilogram, while recovery of the target compounds showed a variation from 85.9% to 116.5%. The observed relative standard deviations, varying from 14% to 82%, indicate good reproducibility of the results. The proposed method's successful application to sample analysis revealed the presence of 26-dichloro-3-methyl-14-benzoquinone (26-DCMBQ) in grass carp specimens. The simultaneous determination of five HBQs in aquatic products is facilitated by this convenient, sensitive, accurate, and suitable method. Furthermore, the established methodology furnishes a dependable benchmark for the ongoing surveillance of trace HBQs in comestible specimens.Drinking water disinfection is vital for the prevention of waterborne diseases. The interaction of disinfectants with organic materials (natural or synthetic) and halides during water disinfection is responsible for the creation of disinfection by-products. These by-products demonstrate significant toxicological and carcinogenic effects. The emerging disinfection by-product, halobenzoquinones (HBQs), has gained increasing attention owing to their severe toxicity and prevalent detection. The accurate assessment of HBQs is essential for advancing research concerning their occurrence, toxicity, and management strategies; however, trace quantities of HBQs are typically found in drinking water. Consequently, precise and effective analytical methods are essential for the establishment of HBQ levels and quantities. A novel method utilizing solid-phase extraction (SPE) in conjunction with ultra-performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS) was developed in this study to quantify 13 halogenated benzoquinones (HBQs) in drinking water. These included six chlorobenzoquinones, six bromobenzoquinones, and one iodobenzoquinone. 25 milliliters of formic acid were added to each one-liter water sample, after which 500 milliliters of each were collected for enrichment purposes. Pretreatment optimization efforts were largely directed towards the SPE column, solvent washing, and nitrogen purging temperature settings. The samples, after being processed using Plexa SPE columns (200 mg/6 mL), were washed with a solution consisting of ultrapure water, 0.25% formic acid, and a 30% methanol aqueous solution, which also incorporated 0.25% formic acid. Then, they were eluted with 6 mL of methanol containing 0.25% formic acid, and finally nitrogen blown at 30°C. Through comparison of results from two reversed-phase columns (BEH C18 and HSS T3), varied formic acid concentrations within the mobile phase, and the establishment of optimal instrumental settings, the UPLC-MS/MS parameters were fine-tuned. An HSS T3 column (100 mm × 21 mm, 18 m) was employed for the gradient elution separation of 13 HBQs over a 16-minute period, utilizing a mobile phase consisting of 0.1% formic acid aqueous solution and methanol. Employing a multiple reaction monitoring (MRM) approach, a triple quadrupole mass spectrometer fitted with a negative electrospray ionization (ESI-) source, was used to detect all 13 HBQs. The quantification of the HBQs was accomplished using matrix-matched calibration curves, a necessity due to the intense matrix inhibitory effects. The results showcased the excellent linear relationships inherent in the 13 HBQs, resulting in correlation coefficients (r) exceeding 0.999. Limits of detection (MDLs, signal-to-noise ratio of 3) for the method fell between 2 and 100 ng/L, while the quantification limits (MQLs, signal-to-noise ratio of 10) lay between 6 and 330 ng/L. Recoveries of the 13 HBQs, spiked at three levels (10, 20, and 50 ng/L), fell between 56% and 88%. Relative standard deviations (RSDs, n=6) were all less than or equal to 92%.