Determination of Sinigrin in Vegetable Seeds by Online Microdialysis Sampling Coupled to Reverse-Phase Ion-Pair Liquid Chromatography

Abstract

A hollow fiber microdialysis sampling coupled online to ion-pair liquid chromatography was investigated as an alternative to sample pretreatment for the direct determination of sinigrin in cruciferous vegetables without desulfation. After microdialysis, the dialysate was online injected into the chromatographic system to analyze the sinigrin with UV detection at 227 nm. Parameters affecting the microdialysis efficiency, such as flow rate, polarity modifier, pH in perfusion stream, pH, and salt added in sample solution, were studied. Through ion suppression in the donor phase and ion-pair formation in the acceptor phase, the microdialysis efficiency of sinigrin was enhanced. Experimental results revealed that the microdialysis of a sample solution (pH 2.0) using 0.1 M tetrabutylammonium (pH 12) as a perfusate at 10 microL/min flow rate maximized the extraction efficiency. Detection was linear in the concentration of 1.0-100 mg/L with a detection limit of 0.3 mg/L. Three seed samples were analyzed, with sinigrin at 49.8 (3.15% RSD), 20.0 (4.43% RSD), and 19.8 mg/g (4.22% RSD) for brussels, cauliflower, and cabbage, respectively. When 40 mg/g sinigrin was spiked in brussels seed powder, the recovery was 102.4% with 3.15% RSD (n = 3). The proposed method was proven to provide a very simple, rapid, and eco-friendly procedure to determine sinigrin in the seeds of cruciferous vegetables.

Sinigrin and Its Therapeutic Benefits

“…Sinigrin has been positively identified by using (1) 1 H-NMR spectroscopy [20]. A hollow fiber microdialysis sampling, coupled to ion pair liquid chromatography, was developed for the direct determination of sinigrin without desulfation [21].…”

Determination of Alachlor and Its Metabolite 2,6-Diethylaniline in Microbial Culture Medium Using Online Microdialysis Enriched-Sampling Coupled to High-Performance Liquid Chromatography

“…The online microdialysis sampling coupled HPLC was assembled with minor modifications as in our previous paper. 29,32,34 A schematic diagram of the online HF-LPME/HPLC-UV system used for determination of alachlor and 2,6-DEA in culture medium is presented in Figure 1b.…”

“…1090 μm), the inlet of the hollow fiber for LPME was connected to a syringe pump containing perfusion solvent and the outlet connected to the sample-loop of a switching valve. The online microdialysis sampling coupled HPLC was assembled with minor modifications as in our previous paper. ,, A schematic diagram of the online HF-LPME/HPLC-UV system used for determination of alachlor and 2,6-DEA in culture medium is presented in Figure b.…”

“…Recently, online microdialysis sampling with HF was established as an LPME technique with high enrichment potential by controlling the status of the sample solution and the conditions of the perfusion stream. − Thus, interference due to the interaction of analyte with sample matrix species can be decreased through the dilution of the sample solution. Online HPLC with HF microdialysis perfusion sampling provides simplified sample preparation and has been successfully applied to biosamples, , cosmetic and polymer wastewater samples, , vegetable seeds, and fermented milk and drinks . However, there is no report related to the application of microdialysis sampling as the cleanup process and enrichment step in the determination of alachlor and its metabolite 2,6-DEA so far.…”

Membrane-Based Extraction Techniques in Food Analysis

“…For instance, fluoroquinolones were separated, utilizing a 15-kDa cellulose probe, in eggs 42 and in chicken liver and muscle, 43 metal ions in tomatoes 44 with a polyethersulfone membrane of 30-kDa cutoff, glucose, galactose, and lactose in milk 45 using a 20-kDa polyarylethersulfone (PAES) probe, catechins in tea 46 with a 13-kDa regenerated cellulose probe, and sinigrin in seeds of cruciferous vegetables (brussels, cauliflower, and cabbage) 47 with a 5-kDa cellulose acetate probe.…”