Application Research Of Phenylalanine-substituted Calix[4]Arene Stationary Phase On The Separation And Determination Of Hazardous Substances In Foods

Calixarenes, following crown ethers and cyclodextrines, are the third generation of macrocyclic molecules used as LC stationary phases. Due to the existing multiplex interactions such as hydrophobic、π-πhydrogen bonding and inclusion et al, calixarene silica-bonded stationary phases show excellent retention characteristics and recognition ability to solutes.In recent years, researches on the chromatographic performance and retention mechanisms of calixarene stationary phases have developed rapidly. However, literatures related to applications of such stationary phases on the separation and determination of substances in real samples are relatively less. In this paper, apllications of phenylalanine-substituted calix[4]arene bonded silica stationary phase (PHE-Cx4) on the determination of hazardous substances in foods were systematically investigated, which would make the study of calixarene stationary phases richer. The following three sections were discussed in this paper.1 The retention mechanism of five sulfonamides on PHE-Cx4 was discussed and one method for simultaneous determination of such five sulfa residues in honey and pork was eatablished. A good linear relationship for five residues was achieved in the range of 0.05μg/mL-5.0μg/mL with R2≥0.9988. The LODs and LOQs were 6 ng/mL-13 ng/mL (S/N=3) and 18 ng/mL-42 ng/mL (S/N=10). The recoveries for honey and pork were 85.3%-98.5% and 79.6%-100% respectively. The method was sensitive、accurate and practical.2 Determination of chloramphenicol residues in honey、duck and lobster was implemented by using PHE-Cx4. A good linear relationship was achieved in the range of 0.1μg/mL-10.0μg/mL with R2=0.9996. The LODs and LOQs were 0.005μg/g (S/N=3) and 0.02μg/g (S/N=10) respectively. The recoveries were 78.2%-93.2% with the RSD%(n=5)between 0.63% and 3.28%. This method was suitable for rapid detection of chloramphenicol residues in real samples.3 Rapid determination of melamine in raw milk、yogurt and milk power was carried out. A good linear relationship was achieved in the range of 0.8μg/ml-80 μg/ml with R2=0.9998. The LODs and LOQs was 0.1μg/g (S/N=3)and 0.34μg/g (S/N=10) respectively. The recoveries were 87.4%-98.4% with the RSD%(n=3) ranging from 0.72% to 3.48%. The sensitivity、accuracy and precision of such method were satisfactory.