Selective extraction and determination of steroidal glycoalkaloids in potato tissues by electromembrane extraction combined with LC-MS/MS.

For the first time, electromembrane extraction (EME) combined LC-MS/MS was applied to extract and determine α-solanine and α-chaconine in different potato tissues using NPOE containing 20% (v/v) DEHP as supported liquid membrane (SLM). Under the optimal conditions, the proposed EME-LC-MS/MS method was evaluated using spiked fresh potato peel sample. The linear range for α-solanine and α-chaconine was 5-1000 ng mL-1 (R2 > 0.9991), with LOD and LOQ of 1.2-1.5 ng mL-1 and 4.1-5.2 ng mL-1, respectively. Repeatability for α-solanine and α-chaconine at three concentration levels was satisfactory (<4.9%), and recoveries ranged from 73% to 106%. Finally, the EME-LC-MS/MS method has been successfully employed to determine α-solanine and α-chaconine in sprouted potato peel and tuber samples, indicating that EME exhibited high selectivity and efficient sample clean-up capability. Consequently, EME showed great potential for extraction and purification of toxic and bioactive basic compounds from complex plant tissues.

Electrocolorimetric gel-based sensing approach for simultaneous extraction, preconcentration, and detection of iodide and chromium (VI) ions.

A total integrated electrocolorimetric sensing approach consisting of gel-based electromembrane extraction and colorimetric detection in a one-step process was developed. This system was designed using colorimetric reagents preadded to the agarose gel for the determination of the following two model analytes: iodide and hexavalent chromium [Cr(VI)]. In this system, when a voltage was applied, the analytes were extracted and transferred from the sample solution (donor phase) to the gel (acceptor phase). The analytes then simultaneously reacted with the colorimetric reagents inside the gel, yielding blue and violet colors for iodide and Cr(VI), respectively. These colors were then analyzed using a portable spectrometer and could also be distinguished with the naked eye. Parameters affecting the extraction efficiency were studied and optimized for both analytes. The gel composition for iodide detection was 4% (w/v) agarose, 5% (v/v) H2O2, and 1% (w/v) starch in 2 mM HCl. The gel composition for Cr(VI) detection was 2% (w/v) agarose and 1% (w/v) DPC in 0.5 mM HNO3. Both analytes were extracted at an applied potential of 50 V, an extraction time of 15 min and a stirring rate of 600 rpm. Under the optimized conditions, the developed systems provided linear responses within 15 min for iodide concentrations ranging from 50 to 250 µg L-1 with a detection limit of 18 µg L-1 and for Cr(VI) concentrations ranging from 30 to 125 µg L-1 with a detection limit of 5 µg L-1. Finally, these systems were successfully applied to the determination of iodide in iodide food supplement samples and Cr(VI) in drinking water samples, showing a negligible matrix effect. This integration could also be extended to other analytes and detection systems to develop sensitive, on-site, and environmentally friendly sensing approaches.

Gel electromembrane microextraction followed by ion chromatography for direct determination of iodine in supplements and fortified food samples: Green chemistry for food analysis.

In this study, a sensitive, selective, and environmentally friendly analytical method for direct extraction and preconcentration of iodine was developed. Iodine, as an iodate ion or iodide ion, was simultaneously extracted and preconcentrated by gel electromembrane microextraction (G-EME) and analyzed for total iodine by ion chromatography. The total iodine was determined by combining the peak areas of both iodate and iodide ions. Under the optimized conditions, linear calibration for iodine using a mixture of iodate and iodide ions was obtained from 10 to 100 µg L-1 (r2 > 0.996). The detection limit was 7.0 µg L-1. Recoveries of spiked iodine (as iodate) in the samples were greater than 90%. The method was applied for the determination of iodine in dietary supplements and fortified food samples, i.e., iodine-enriched eggs. Our developed method could be directly applied for the determination of iodine in different matrix samples including eggs without a pretreatment step.

Electromembrane extraction of aristolochic acids: New insights in separation of bioactive ingredients of traditional Chinese medicines.

Aristolochic acid (AA) I and AA II, which have been classified as carcinogenic to human and have been proven to be nephrotoxic, are bioactive ingredients of many traditional Chinese medicines (TCMs). Thus, development of an efficient approach for separation and determination of AA I and AA II in biological samples and herbal plants is of significance. Herein, electromembrane extraction (EME) was for the first time used to separate AA I and AA II. It is noted that also for the first time 1-decanol was discovered and used as an efficient SLM solvent for EME of acidic compounds. The proposed EME system was used to extract AA I and AA II from urine samples (recovery≥68%). The approach of EME combined with LC-MS (EME-LC/MS) was evaluated using urine samples. The linear range for AA I and AA II was 10-1000 ng mL-1 (R2≥0.9970), and the limits of detection (LOD, S/N = 3) for AA I and AA II were 2.7 and 2.9 ng mL-1, respectively. Finally, this EME-LC/MS approach was employed to discover AA I and AA II in the herbal plants. In addition, using standard addition method, AA I in Aristolochicaceae-Liao Asarum (ALA) and Radix Aristolochice (RA) were 0.23 and 2044.13 µg g-1, and AA II in ALA and RA were 0 and 338.48 µg g-1, respectively. The repeatability of EME-LC/MS at all cases for both urine samples and herbal plants was below 15% (RSD-value). We believe that EME would be a useful tool to isolate bioactive ingredients of TCMs from complex samples for different purposes.