scholarly journals Poly (Octadecyl Methacrylate-Co-Trimethylolpropane Trimethacrylate) Monolithic Column for Hydrophobic in-Tube Solid-Phase Microextraction of Chlorophenoxy Acid Herbicides

Molecules ◽  
2019 ◽  
Vol 24 (9) ◽  
pp. 1678 ◽  
Author(s):  
Wenbang Li ◽  
Fangling Wu ◽  
Yongwei Dai ◽  
Jing Zhang ◽  
Bichen Ni ◽  
...  

Chlorophenoxy acid herbicides (CAHs), which are widely used on cereal crops, have become an important pollution source in grains. In this work, a highly hydrophobic poly (octadecyl methacrylate-co-trimethylolpropane trimethacrylate) [poly (OMA-co-TRIM)] monolithic column has been specially prepared for hydrophobic in-tube solid-phase microextraction (SPME) of CAHs in rice grains. Due to the hydrophobicity of CAHs in acid conditions, trace CAHs could be efficiently extracted by the prepared monolith with strong hydrophobic interaction. Several factors for online hydrophobic in-tube SPME, including the length of the monolithic column, ACN and trifluoroacetic acid percentage in the sampling solution, elution volume, and elution flow rate, were investigated with respect to the extraction efficiencies of CAHs. Under the optimized conditions, the limits of detection of the four CAHs fell in the range of 0.9–2.1 μg/kg. The calibration curves provided a wide linear range of 5–600 μg/kg and showed good linearity. The recoveries of this method ranged from 87.3% to 111.6%, with relative standard deviations less than 7.3%. Using this novel, highly hydrophobic poly (OMA-co-TRIM) monolith as sorbent, a simple and sensitive online in-tube SPME-HPLC method was proposed for analysis of CAHs residue in practical samples of rice grains.

Molecules ◽  
2020 ◽  
Vol 25 (4) ◽  
pp. 897 ◽  
Author(s):  
Qian-Chun Zhang ◽  
Guang-Ping Xia ◽  
Jun-Yi Liang ◽  
Xiao-Lan Zhang ◽  
Li Jiang ◽  
...  

In this study, a novel monolithic capillary column based on a NH2-MIL-53(Al) metal–organic framework (MOF) incorporated in poly (3-acrylamidophenylboronic acid/methacrylic acid-co-ethylene glycol dimethacrylate) (poly (AAPBA/MAA-co-EGDMA)) was prepared using an in situ polymerization method. The characteristics of the MOF-polymer monolithic column were investigated by scanning electron microscopy, Fourier-transform infrared spectroscopy, X-ray photoelectron spectroscopy, X-ray diffractometry, Brunauer-Emmett-Teller analysis, and thermogravimetric analysis. The prepared MOF-polymer monolithic column showed good permeability, high extraction efficiency, chemical stability, and good reproducibility. The MOF-polymer monolithic column was used for in-tube solid-phase microextraction (SPME) to efficiently adsorb trace sulfonamides from food samples. A novel method combining MOF-polymer-monolithic-column-based SPME with ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was successfully developed. The linear range was from 0.015 to 25.0 µg/L, with low limits of detection of 1.3–4.7 ng/L and relative standard deviations (RSDs) of < 6.1%. Eight trace sulfonamides in fish and chicken samples were determined, with recoveries of the eight analytes ranging from 85.7% to 113% and acceptable RSDs of < 7.3%. These results demonstrate that the novel MOF-polymer-monolithic-column-based SPME coupled with UHPLC-MS/MS is a highly sensitive, practical, and convenient method for monitoring trace sulfonamides in food samples previously extracted with an adequate solvent.


2016 ◽  
Vol 81 (8) ◽  
pp. 923-934 ◽  
Author(s):  
Rada Djurovic-Pejcev ◽  
Tijana Djordjevic ◽  
Vojislava Bursic

A method is described for simultaneous determination of five herbicides (metribuzin, acetochlor, clomazone, oxyfluorfen and dimethenamid) belonging to different pesticides groups in soil samples. Developed headspace solid phase microextraction method (HS-SPME) in combination with liquid-solid sample preparation (LS) was optimized and applied in the analysis of some agricultural samples. Optimization of microextraction conditions, such as temperature, extraction time and sodium chloride (NaCl) content was perfor-med using 100 ?m polydimethyl-siloxane (PDMS) fiber. The extraction effi-ciencies of methanol, methanol:acetone=1:1 and methanol:acetone:hexane= =2:2:1 and the optimum number of extraction steps during the sample prepa-ration, were tested, as well. Gas chromatography-mass spectrometry (GC-MS) was used for detection and quantification, obtaining relative standard deviation (RSD) below 13%, and recovery values higher than 83% for multiple analyses of soil samples fortified at 30 ?g kg-1 of each herbicide. Limits of detection (LOD) were less than 1.2 ?g kg-1 for all the studied herbicides.


Author(s):  
Huiju Wang

Ionic     liquid (IL), 1-dodecyl-3-methylimidazolium-3-hydroxy-2-naphthoate (C12mimHNC) was synthesized and coated on the surface of NiTi as solid phase microextractiom fiber coating for determination the octadecylamine in brine. Prior to modification with IL, the NiTi was hydrothermally treated for in-situ growth of titanium and nickel oxide composite nanosheets (TiO2/NiOCNSs). The TiO2/NiOCNSs fibers coating was oriented  around the NiTi  substrate and  presented  double-faced  open  access  sites,  which provided a desired support framework for the further modification with IL. The extraction performance of C12mimHNC-TiO2/NiOCNSs fiber coating was evaluated for       detection of octadecylamine (ODA) coupled to HPLC with UV detection. As a result, the C12mimHNC-TiO2/NiOCNSs fiber coating illustrated excellent adsorption and extraction capability for ODA. The main factors affected extraction efficiency were optimized. Under the optimized  conditions,  good  linearity was  obtained  in  the  range of  1-150  µg/L with correlation  coefficients  (r2)  above  0.985.  Limits of detection (LODs) for  the  developed method was 0.280 µg/L. The proposed method was first applied to extract the ODA in brine samples. Relative recoveries varied from 78.3% to 96.5% at spiking level of 15µg/L and 30 µg/L with the relative standard deviations (RSDs) less than 8.7%.


RSC Advances ◽  
2014 ◽  
Vol 4 (90) ◽  
pp. 49153-49160 ◽  
Author(s):  
Dan Liu ◽  
Nan Song ◽  
Ye-Chun Cheng ◽  
Dai-Xiong Chen ◽  
Qiong Jia ◽  
...  

2009 ◽  
Vol 92 (3) ◽  
pp. 855-861 ◽  
Author(s):  
Tao Zhou ◽  
Bei Yang ◽  
Haiying Zhang ◽  
Yingjia Yu ◽  
Bin Chen ◽  
...  

Abstract Microwave distillation with concomitant solid-phase microextraction (MD-SPME) coupled with GC/MS was developed for identifying volatile compounds in the dried flowers of Chrysanthemum morifolium (CM). Different experimental parameters, including SPME fiber coating, microwave power, irradiation time, and water volume were optimized. The best results were obtained using carboxen/polydimethylsiloxane fiber with microwave irradiation at 400 W for 3 min and the addition of 1 mL water into 1.0 g sample. The proposed method allowed the isolation, extraction, and concentration of volatile compounds to be completed in a single step. This MD-SPME-GC/MS method has also been compared to the conventional steam distillation method followed by GC/MS for this identification. Thirty-two volatile compounds were identified using the newly developed MD-SPME-GC/MS process. Relative standard deviation values of &lt;9.8 demonstrate good repeatability. In comparison, 27 compounds were identified by traditional steam distillation-GC/MS. Therefore, the proposed MD-SPME-GC/MS method is simple, rapid, and efficient for identifying volatile compounds in CM.


Molecules ◽  
2019 ◽  
Vol 24 (9) ◽  
pp. 1670 ◽  
Author(s):  
Sandip Mondal ◽  
Jialing Jiang ◽  
Yin Li ◽  
Gangfeng Ouyang

In this study, the detection and quantification of multiple classes of antibiotics in water matrices are proposed using a lab-made solid phase microextraction (SPME) fiber coupled with high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). The lab-made fiber was prepared using a graphene oxide (G), carbon nanotubes (C), and tin dioxide (T) composite, namely GCT, with polyacrylonitrile (PAN) as supporting material. The detected antibiotics were enrofloxacin, sulfathiazole, erythromycin, and trimethoprim. The custom-made fiber was found to be superior compared with a commercial C18 fiber. The excellent reproducibility and lower intra-fiber relative standard deviations (RSDs 1.8% to 6.8%) and inter-fiber RSDs (4.5% to 8.8%) made it an ideal candidate for the detection of traces of antibiotics in real environmental samples. The proposed validated method provides a satisfactory limit of detection and good linear ranges with higher (>0.99) coefficient of determination in the aqueous system. Application of the method was made in different real water systems such as river, pond and tap water using the standard spiking method. Excellent sensitivity, reproducibility, lower amount of sample detection and higher recovery was found in a real water sample. Therefore, the extraction method was successfully applied to the detection and quantification of multiple classes of antibiotics in different aqueous systems with satisfactory results.


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