scholarly journals Sulfonic Acid-Functionalized SBA-15 as Strong Cation-Exchange Sorbent for Solid-Phase Extraction of Atropine and Scopolamine in Gluten-Free Grains and Flours

Foods ◽  
2020 ◽  
Vol 9 (12) ◽  
pp. 1854
Author(s):  
Lorena González-Gómez ◽  
Judith Gañán ◽  
Sonia Morante-Zarcero ◽  
Damián Pérez-Quintanilla ◽  
Isabel Sierra
Keyword(s):  
Solid Phase Extraction ◽  
Cation Exchange ◽  
Solid Phase ◽  
Tropane Alkaloids ◽  
Sample Treatment ◽  
Phase Extraction ◽  
Gluten Free ◽  
Strong Cation Exchange ◽  
Sorghum Flour ◽  
Solid Liquid

A novel method was developed and applied to the determination of the most representative tropane alkaloids (TAs), atropine and scopolamine, in gluten-free (GF) grains and flours by HPLC-MS/MS. Accordingly a suitable sample treatment procedure based on solid-liquid extraction (SLE) and followed by strong cation-exchange solid-phase extraction (SCX-SPE) was optimized. SBA-15 mesostructured silica functionalized with sulfonic acids was evaluated as sorbent. The proposed method was fully validated in sorghum flour showing good accuracy with recoveries in the range of 93–105%, good linearity (R2 > 0.999) and adequate precision (RSD < 20%). Low method quantification limits (MQL) were obtained (1.5 and 2.4 µg/kg for atropine and scopolamine, respectively) and no matrix effect was observed thanks to the extraction and clean-up protocol applied. The method was applied to 15 types of GF samples of pseudocereals (buckwheat, quinoa and amaranth), cereals (teff, corn and blue corn, sorghum and millet) and legumes (red and green lentil, chickpea and pea). Atropine was found above the MQL in eight of them, with values between 7 and 78 µg/kg, while scopolamine was only found in teff flour, its concentration being 28 µg/kg. The method developed is an interesting tool for determining TAs in a variety of samples of GF grains and flours.

Liquid Chromatographic Determination of the Cyanobacterial Toxin β-N-Methylamino-L-Alanine in Algae Food Supplements, Freshwater Fish, and Bottled Water

2009 ◽  
Vol 72 (8) ◽  
pp. 1769-1773 ◽  
Author(s):  
PETER M. SCOTT ◽  
BARBARA NIEDZWIADEK ◽  
DOROTHEA F. K. RAWN ◽  
BEN P.-Y. LAU
Keyword(s):  
Solid Phase Extraction ◽  
Cation Exchange ◽  
Freshwater Fish ◽  
Solid Phase ◽  
Bottled Water ◽  
Extraction Column ◽  
Phase Extraction ◽  
Solid Phase Extraction Column ◽  
Strong Cation Exchange

β-N-Methylamino-l-alanine (BMAA) is a neurotoxin originally found in cycad seeds and now known to be produced by many species of freshwater and marine cyanobacteria. We developed a method for its determination in blue-green algae (BGA) food supplements, freshwater fish, and bottled water by using a strong cation-exchange, solid-phase extraction column for cleanup after 0.3 M trichloroacetic acid extraction of BGA supplements and fish. Bottled water was applied directly onto the solid-phase extraction column. For analysis of carbonated water, sonication and pH adjustment to 1.5 were needed. To determine protein-bound BMAA, the protein pellet left after extraction of the BGA supplement and fish was hydrolyzed by boiling with 6 M hydrochloric acid; BMAA was cleaned up on a C18 column and a strong cation-exchange, solid-phase extraction column. Determination of BMAA was by liquid chromatography of the fluorescent derivative formed with 9-fluorenylmethyl chloroformate. The method was validated by recovery experiments using spiking levels of 1.0 to 10 μg/g for BGA supplements, 0.5 to 5.0 μg/g for fish, and 0.002 μg/g for bottled water; mean recoveries were in the range of 67 to 89% for BGA supplements and fish, and 59 to 92% for bottled water. Recoveries of BMAA from spiked extracts of hydrolyzed protein from BGA supplements and fish ranged from 66 to 83%. The cleanup developed provides a useful method for surveying foods and supplements for BMAA and protein-bound BMAA.

Sign in / Sign up

Export Citation Format

Share Document