Trace Sulfonamides Research Articles

A novel metal-organic framework composite MIL-101(Cr)@GO as an efficient sorbent in dispersive micro-solid phase extraction coupling with UHPLC-MS/MS for the determination of sulfonamides in milk samples

As a novel material, metal-organic framework/graphite oxide (MIL-101(Cr)@GO) has great potential for the pretreatment of trace analytes. In the present study, MIL-101(Cr)@GO was synthesized using a solvothermal synthesis method at the nanoscale and was applied as sorbent in the dispersive micro-solid phase extraction (DMSPE) for the enrichment of the trace sulfonamides (SAs) from milk samples for the first time. Several experimental parameters including kinds of sorbents, the effect of pH, the amount of MIL-101(Cr)@GO, ionic strength, adsorption time, desorption solvent and desorption time were investigated. Under the optimal conditions, the linear ranges were from 0.1 to 10μg/L, 0.2–20μg/L or 0.5–50μg/L for the analytes with regression coefficients (r) from 0.9942 to 0.9999. The limits of detection were between 0.012 and 0.145μg/L. The recoveries ranged from 79.83% to 103.8% with relative standard deviations (RSDs)<10% (n=3). MIL-101(Cr)@GO exhibited remarkable advantages compared to MIL-101(Cr), MIL-100(Fe), activated carbon and other sorbent materials used in pretreatment methods. A simple, rapid, sensitive, inexpensive and less solvent consuming method of DMSPE-ultra-high performance liquid chromatography-tandem mass spectrometry (DMSPE-UHPLC-MS/MS) was successfully applied to the pre-concentration and determination of twelve SAs in milk samples.

Determination of Sulfonamides in Fish Using a Modified QuEChERS Extraction Coupled with Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry

In the present work, an improved QuEChERS (quick, easy, cheap, effective, rugged and safe) protocol coupled with ultra-performance liquid chromatography-tandem mass spectrometry analytical method was developed and validated for determination of trace sulfonamides residues in fish tissues. The QuEChERS protocol was modified in terms of extraction solvent, as well as a graphene-based dispersive solid-phase cleanup procedure. Some extraction conditions such as solvent, acidity, and the amount of graphene sorbent were evaluated. The matrix effect related to the QuEChERS extraction from fish tissues was studied and compared with conventional QuEChERS protocol. The target analytes were quantified by a triple-quadrupole linear ion-trap mass spectrometer in multiple-reaction monitoring mode. The matrix-matched calibration curves were performed at seven concentration levels and good linear relationship (R2 > 0.999) was observed within the range of 0.5–200 μg kg −1. Recoveries of the spiked samples ranged between 70.7 and 100.9 % with relative standard deviation lower than 9.2 %. The limits of quantification were between 2.62 and 9.03 μg kg−1. The method was successfully applied to the analysis of real samples.

Rapid Determination of Trace Sulfonamides in Milk by Graphene Oxide-Based Magnetic Solid Phase Extraction Coupled with HPLC–MS/MS

A simple and rapid method based on magnetic solid-phase extraction (MSPE) combined with high-performance liquid chromatography coupled with triple quadrupole mass spectrometry (HPLC–MS/MS) was used for the determination of 15 sulfonamides from milk samples. The extraction and cleanup used a graphene oxide-based magnetic nanocomposite (Fe3O4@GO) as an adsorbent. Various experimental parameters that could affect the extraction efficiencies, such as the amount of Fe3O4@GO, the extraction time, the ionic strength of sample solution, and the type of eluent, were investigated. Under optimized experimental conditions, good linearity was observed in the range of 2.0 to 100.0 μg L−1 for all of the analytes, with correlation coefficients (R2) ranging from 0.994 to 0.999. The limits of detection for the method ranged between 0.02 and 0.13 μg L−1. Mean values of the relative standard deviation of intraday and interday precision ranging from 1.0 to 7.3 % and from 1.7 to 8.1 % were obtained, respectively. The average recoveries were between 73.4 and 97.4 % at three different spiked levels. It was confirmed that the Fe3O4@GO nanocomposite was an effective MSPE material for use in sulfonamide analyses in milk samples.

Determination of trace sulfonamides in foodstuffs by HPLC using a novel mixed-mode functionalized ferrocene sorbent for solid-phase extraction cleanup

In this paper, a rapid and effective HPLC method, using a new 4-chloro-6-pyrimidinylferrocene-modified silica gel (NFcSi) as a solid-phase extraction (SPE) sorbent, was developed for the purification and determination of trace sulfonamides in foodstuffs.

Magnetite–graphene oxide composites as a magnetic solid-phase extraction adsorbent for the determination of trace sulfonamides in water samples

Magnetite–graphene oxide composites were used for magnetic solid-phase extraction to preconcentrate trace sulfonamides in water samples before determination by high-performance liquid chromatography.

Hollow-fiber liquid-phase microextraction combined with capillary electrophoresis for trace analysis of sulfonamide compounds

A hollow-fiber liquid-phase microextraction (HF-LPME) method has been developed for the preconcentration of trace sulfonamides in water samples. Six commonly used sulfonamides including sulfamethazine (SMZ), sulfamerazine (SMR), sulfadiazine (SDZ), sulfadimethoxine (SDM), sulfamethoxazole (SMX), and sulfathiazole (STZ) were determined by CE with electrochemical detection (CE-ED) after microextraction. Several factors that affect extraction efficiency, separation, and detection were investigated. Under the optimum conditions, above sulfonamide compounds could achieve baseline separation within 35min, exhibiting a linear calibration over three orders of magnitude (r(2)≥0.998); the obtained enrichment factors were between 121 (for SDZ) and 996 (for SDM), and the LODs were in the range of 0.033-0.44ng/mL. The proposed HF-LPME/CE-ED method has been applied for the sensitive analyses of the real-world water samples with recoveries in the range of 75.1-109%.

The Ion Chromatography Intergrated Amperometry Method to Detectsulfonamides

In this study, the high performance ion chromatography integrated pulsed amperometric detection (HPIC-IPAD) was appliedfor the first time to detect 10 sulfonamides. In this experiment,we used Dionex AS18 (250mm×2mm) and AG18 (50mm×2mm) columnsfilled with an anion exchange resin, with 14 mmol / L NaOH solution concentration. The Analysis temperature was 30 ° C, the flow rate was 0.25 mL / min, and the injection volume was 10 μL. The detection was through pulsed amperometric detection cell with Au electrode and reference electrode pH-Ag/AgCl as working electrodes. Take the standard stock solution compounding 0.06,0.15,0.30,1.5,3.0 mg / L standard solutions respectively,build linear regression on chromatographic peak area as Y and analyte mass concentration of as X (mg / L). In the range of 0.06-3.0 mg / L, the 10 sulfonamides response appeared a linear relationship (R&gt; 0.9989). This method can be considered for the detection of trace sulfonamides substances in cosmetics, food, and feed.

Rapid determination of trace sulfonamides in fish by graphene-based SPE coupled with UPLC/MS/MS

An analytical protocol for simultaneous determination of thirteen sulfonamides in fish tissues has been developed. Target analytes were enriched by solid-phase extraction using graphene as a sorbent and quantified by ultra-high-performance liquid chromatography coupled with triple-quadrupole linear ion trap mass spectrometry. In the present work, graphene was systematically evaluated as a solid-phase extraction sorbent for analyte enrichment and clean-up. Under optimized conditions, average recoveries of individual sulfonamides were between 76.2 and 91.5% at three different spiked levels, the matrix-matched calibration curves were prepared at six concentration levels and a good linear relationship (R2 > 0.990) was observed. The mean values of relative standard deviation of intra- and inter-day precision ranging from 1.8 to 5.7% and from 2.9 to 7.6% were obtained, respectively. The proposed method has been successfully applied to the analysis of sulfonamides in grass carp fish samples, indicating the potential of graphene as a SPE sorbent for the enrichment of trace residues in food matrices.

Preparation of Trimethoprim Molecularly Imprinted Stir Bar Sorptive Extraction and Its Application for Trace Analysis of Trimethoprim and Sulfonamides in Complex Samples

Abstract Trimethoprim molecularly imprinted polymer (MIP) was prepared as the coating of stir bar sorptive extraction (SBSE) and applied to the trace analysis of trimethoprim and three sulfonamides in complex samples. The MIP-coating was about 21.5 μm thickness with the relative standard deviations (RSD) of 5.9% ( n = 10). It was homogeneous and dense with good thermal and chemical stability. The extraction capability of the MIP-coating was 1.7 times over that of the non-imprinted polymer (NIP) coating. The MIP-coating exhibited selective adsorption ability to sulfonamides, triazines and methotrexate besides antibacterial synergists. The methods for the determination of trimethoprim and three sulfonamides by MIP-coated stir bar sorptive extraction coupled with HPLC were developed. It was successfully applied to the trace trimethoprim analysis in spiked urine and plasma samples. The linear range was 5-200 μg L −1 and the detection limit was 1.6 μg L −1 . The recoveries in urine and plasma samples were 84.5% to 91.7% with RSDs of 2.9%–4.4%, 71.9% to 85.1% with RSDs of 3.0%–7.3%, respectively. The trimethoprim MIP-coated stir bar was also applied to the trace sulfonamides analysis in spiked milk sample. The linear range was 10–200 μg L −1 , the detection limit was within the range of 4.5–6.1 μg L −1 , and the recovery was 83.2%–110.2% with RSDs of 4.1%–8.0%.

Molecularly Imprinted Polymer Online Solid-Phase Extraction Coupled with High-Performance Liquid Chromatography−UV for the Determination of Three Sulfonamides in Pork and Chicken

A selective imprinted amino-functionalized silica gel sorbent was prepared by combining a surface molecular imprinting technique with a sol-gel process for online solid-phase extraction-HPLC determination of three trace sulfonamides in pork and chicken muscle. The imprinted functionalized silica gel sorbent exhibited selectivity and fast kinetics for the adsorption and desorption of sulfonamides. With a sample loading flow rate of 4 mL min (-1) for 12.5 min, enhancement factors and detection limits for three sulfonamides ( S/ N = 3) were achieved. The precision (RSD) for nine replicate online sorbent extractions of 5 microg L (-1) sulfonamides was less than 4.5%. The sorbent also offered good linearity ( r (2) > 0.99) for online solid-phase extraction of trace levels of sulfonamides. The method was applied to the determination of sulfonamides in pork and chicken muscle samples. The prepared polymer sorbent shows promise for online solid-phase extraction for HPLC determination of trace levels of sulfonamides in pork and chicken samples.

Trace determination of sulfonamides residues in meat with a combination of solid-phase microextraction and liquid chromatography–mass spectrometry

An integrated method of combining solid-phase microextraction (SPME) with liquid chromatography–mass spectrometry (LC–MS) was evaluated for determination trace amount of sulfonamides in meat products. Eight commonly used sulfonamides, sulfadiazine (SDZ), sulfathiazole (STZ), sulfamerazine (SMR), sulfamethazine (SMT), sulfamonomethoxine (SMMX), sulfamethoxazole (SMXZ), sulfaquinoxaline (SQX) and sulfadimethoxine (SDMX), were investigated in this study. Chromatography was performed on a C 18 reversed-phase column using an isocratic acetonitrile in water as the mobile phase. Fiber coated with a 65 μm thickness of polydimethylsiloxane/divinylbenzene (PDMS/DVB) was used to extract sulfonamides at optimum conditions. Analytes were desorbed with static desorption in an SPME-HPLC desorbed chamber for 15 min and then determined by LC–MS. The detection limits of these sulfonamides in pork were from 16 μg kg −1 (SMT) to 39 μg kg −1 (SMMX). According to the analysis, the linear range was from 50 to 2000 μg kg −1 with relative standard deviation (R.S.D.s) value below 15% (intra-day) and 19% (inter-day). The proposed method was tested by analyzing meats from a local market for sulfonamides residues. Some sulfonamides in our study were detected in the meat samples. The concentration of these residual sulfonamides ranged from 66 μg kg −1 (SDZ) to 157 μg kg −1 (SQX) in a chicken sample. The results demonstrate that the SPME–LC–MS system is highly effective in analyzing trace sulfonamides in meat products.