scholarly journals SPE-UHPLC-FLD Method for the Simultaneous Determination of Five Anthraquinones in Human Urine Using Mixed-Mode Bis(tetraoxacalix[2]arene[2]triazine) Modified Silica as Sorbent

2017 ◽  
Vol 2017 ◽  
pp. 1-10 ◽  
Author(s):  
Kai Hu ◽  
Yonghui Qiao ◽  
Zhifen Deng ◽  
Mingxia Wu ◽  
Wei Liu
Keyword(s):  
Human Urine ◽  
Mixed Mode ◽  
Solid Phase ◽  
Herbal Medicines ◽  
Correlation Coefficients ◽  
Modified Silica ◽  
Modified Silica Gel ◽  
Aloe Emodin ◽  
Spe Method

The five anthraquinones compounds (including aloe-emodin, emodin, physcion, chrysophanol, and rhein) are regarded as the main effective ingredients in rhubarb (Dahuang in Chinese, one of the commonly used Chinese herbal medicines). In this work, a simple and effective solid phase extraction (SPE) method based on bis(tetraoxacalix[2]arene[2]triazine) modified silica gel as adsorbent was developed. Coupled with UHPLC-FLD, the developed method was successfully applied for the measuring of main anthraquinones in human urine after oral administration of the extracts of rhubarb. To obtain the highest recoveries of the five anthraquinones in the SPE process, the main parameters which may affect extraction efficiency were optimized. The optimized sorbent amount, sample loading pH, sample loading rate, washing solution, and eluent condition were obtained. The developed method showed good linearity in 0.012–1.800 μg mL−1 for the five anthraquinones with correlation coefficients more than 0.9993. The investigated LOD values ranged from 3.9 to 5.7 ng mL−1, while the LOQs were between 12.0 and 18.2 ng mL−1. The recoveries of the method were also investigated, which were in the range of 94.8–106.6%. The application of the mixed-mode SPE materials in the proposed method was feasible and simple, and suitable for the enrichment of anthraquinones in urine samples.

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

2016 ◽  
Vol 8 (31) ◽  
pp. 6099-6106 ◽  
Author(s):  
Lijun Qiao ◽  
Xiaohua Zhou ◽  
Yanhao Zhang ◽  
Ajuan Yu ◽  
Shusheng Zhang ◽  
...  
Keyword(s):  
Solid Phase Extraction ◽  
Silica Gel ◽  
Mixed Mode ◽  
Solid Phase ◽  
Hplc Method ◽  
Phase Extraction ◽  
Modified Silica ◽  
Modified Silica Gel

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.

Direct Determination of Glyphosate and its Metabolite AMPA in Soil Using Mixed-Mode Solid-Phase Purification and LC-MS/MS Determination on a Hypercarb Column

2019 ◽  
Vol 102 (3) ◽  
pp. 952-965 ◽  
Author(s):  
Pei Zhang ◽  
Mick Rose ◽  
Lukas Van Zwieten
Keyword(s):  
Mixed Mode ◽  
Crop Production ◽  
Solid Phase ◽  
Direct Determination ◽  
Correlation Coefficients ◽  
Grain Production ◽  
Internal Standards ◽  
Aminomethylphosphonic Acid ◽  
Lc Tandem Ms

Abstract Background: Although glyphosate is widely used in agriculture, information on its residue level in soils remains scarce partly because of the difficulty in its analysis. Objective: Develop and validate a method to directly analyze glyphosate and its metabolite aminomethylphosphonic acid (AMPA) in soil. Method: Soils were extracted with 0.6 M KOH solution, and coextracted interferences were removed using a mixed-mode Bond Elut Plexa PAX®. The extracts were analyzed by LC-tandem MS fitted with a Hypercarb column and isotope-labeled (13C,15N) glyphosate and AMPA were used as internal standards. Results: LOQs were 0.05 mg/kg for both glyphosate and AMPA in soils. Correlation coefficients were ≥0.99, residuals were below 20%, and calibrations were linear in the range 0.02–1.0 μg/mL. The method was validated on five contrasting soils (Vertosol, Calcarosol, Chromosol, Sodosol, and Tenosol) commonly used for grain production in Australia. The recoveries for glyphosate and AMPA in the soils were 96–121 and 91–118%, respectively, with RSD in the range of 3–16%. Conclusions: This paper presents using the validated method in analysis glyphosate and AMPA in soils collected from crop production paddocks in Australia. The survey data showed that glyphosate and AMPA were detected in all collected soils, with concentrations ranging between 0.05 and 1.2 mg/kg. Highlights: The study demonstrates that the mixed-mode solid-phase extraction is effective in removing interferences and validates the use of Hypercarb as an alternative stationary phase for glyphosate and AMPA analysis from soils.

Preconcentration and determination of Cu(II) in a fresh water sample using modified silica gel as a solid-phase extraction adsorbent

2010 ◽  
Vol 175 (1-3) ◽  
pp. 399-403 ◽  
Author(s):  
A.S. Pereira ◽  
G. Ferreira ◽  
L. Caetano ◽  
M.A.U. Martines ◽  
P.M. Padilha ◽  
...  
Keyword(s):  
Solid Phase Extraction ◽  
Water Sample ◽  
Fresh Water ◽  
Silica Gel ◽  
Solid Phase ◽  
Phase Extraction ◽  
Modified Silica ◽  
Modified Silica Gel

scholarly journals Development and Validation of QuEChERS Followed by UHPLC-ToF-MS Method for Determination of Multi-Mycotoxins in Pistachio Nuts

Molecules ◽  
2021 ◽  
Vol 26 (19) ◽  
pp. 5754
Author(s):  
Ana Rita Soares Mateus ◽  
Sílvia Barros ◽  
Angelina Pena ◽  
Ana Sanches Silva
Keyword(s):  
High Performance ◽  
Solid Phase ◽  
Quechers Method ◽  
Modified Silica ◽  
Modified Silica Gel ◽  
Flight Mass Spectrometry ◽  
High Lipid ◽  
Commission Regulation ◽  
Tof Ms

Pistachios are one of the types of tree nut fruits with the highest mycotoxin contamination, especially of aflatoxins, worldwide. This study developed a Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method that was followed by Ultra-High Performance Liquid Chromatography combined with Time-of-Flight Mass Spectrometry (UHPLC–ToF-MS) for the determination of mycotoxins in pistachios. Different approaches to dispersive solid phase extraction as a clean-up method for high lipid matrices were evaluated. For this, classic sorbents such as C18 (octadecyl-modified silica) and PSA (primary secondary amine), and new classes of sorbents, namely EMR-Lipid (enhanced matrix removal-lipid) and Z-Sep (modified silica gel with zirconium oxide), were used. The QuEChERS method, followed by Z-Sep d-SPE clean-up, provided the best analytical performance for aflatoxins (AFB1, AFB2, AFG1 and AFG2), ochratoxin A (OTA), zearalenone (ZEA), toxin T2 (T2) and toxin HT-2 (HT2) in pistachios. The method was validated in terms of linearity, sensitivity, repeatability, interday precision and recovery; it achieved good results according to criteria imposed by Commission Regulation (EC) no. 401/2006. The method was applied to real samples and the results show that pistachios that are available in Portuguese markets are safe from mycotoxins that are of concern to human health.

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