Determination of Sulfonamides in Propolis by Gas Chromatography/Mass Spectrometry

• Main Authors: ching-ting lee, 李建廷
• Other Authors: Maw-Rong Lee
• Format: Others
• Language: zh-TW
• Published: 2005
• Online Access: http://ndltd.ncl.edu.tw/handle/66893458522264775624

碩士 === 國立中興大學 === 化學系 === 93 === Abstract This study investigates the trace residue of sulfonamides in propolis by using gas chromatography / mass spectrometry ( GC/MS ). Solid phase extraction (SPE) was used for sample pretreatment. The optimal parameters of solid phase extraction including the kind of sorbent, elution solvent and elution volume of solvent were studied. Various derivatization methods such as methylation with diazomethane and acylation with heptafluorobutyric anhydride, trifluoroacetoic anhydride and pentafluoropropionic anhydride were evaluated to derivatize the trace sulfonamides. From the experimental results show that the largest recoveries for sulfonamides were achieved with C8 sorbent and acetonitrile as the eluting solvent at 1 mL/min. The recoveries of sulfonamides were obtained from 83% to 95%. Microwave assisted derivatization with pentafluoropropionic anhydride (PFPA) at 150 Watt for 20 second were obtained to improve the derivatization efficiency. The linearity was obtained with a precision below 7% RSD for the studied sulfonamides. Detection limits were reached at low ng/mL for SPD (sulfapyridine) at 10 ng/mL, SMR (sulfamerazine) at 20 ng/mL, SMT (sulfamethazine) at 6 ng/mL and SME (5-methoxysulfadiazine) at 0.7μg/mL. The results demonstrate the suitability of the technology approach for the analysis of sulfonamides in propolis.