{Reference Type}: Journal Article {Title}: Determination of chloropropanol esters and glycidyl esters in nutritional foods by gas chromatography-tandem mass spectrometry based on acid hydrolysis and solid-phase extraction. {Author}: Li Y;Chen D;Fu W;Yang Y;Chen H;Ni L;Chen H;Jiang D;Zhang S;Gui R; {Journal}: Food Addit Contam Part A Chem Anal Control Expo Risk Assess {Volume}: 41 {Issue}: 7 {Year}: 2024 Jul 28 {Factor}: 3.549 {DOI}: 10.1080/19440049.2024.2353796 {Abstract}: This study presents a method based on acid transesterification and the purification by solid-phase extraction (SPE) coupled with gas chromatography-tandem mass spectrometry for quantifying 3- and 2-monochloropropanediol esters (3-MCPDE, 2-MCPDE) and glycidyl esters (GE) in nutritional foods. The fat was extracted by liquid-liquid extraction with petroleum ether and diethyl ether after the sample was hydrolysed with ammonia. Then the extract was purified by a SPE cartridge filled with the aminopropyl sorbents. It was demonstrated that the optimal elution volume for 3-MCPDE, 2-MCPDE and GE greatly depended on the sample matrix and varied from 6 to 12 mL for four different kinds of food matrices. All three analytes in the sample solution could be fully collected in the first 10-12 mL of eluate. By this way, monoacylglycerols commonly present in the samples were fully removed. Therefore, the overestimation of GE quantification was effectively eliminated. The modified analytical procedure was fully validated in a single laboratory and has been recommended as a Chinese Food Safety National Standard. In addition, two derivatisation agents, heptafluorobutyrylimidazole and phenylboronic acid, were proved to be equivalent in method accuracy and precision for the quantification of three analytes.