Journal
JOURNAL OF CHROMATOGRAPHIC SCIENCE
Volume 58, Issue 5, Pages 471-476Publisher
OXFORD UNIV PRESS INC
DOI: 10.1093/chromsci/bmaa001
Keywords
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Funding
- National Natural Science Foundation of China [31871763]
- Open Foundation of Beijing Advanced Innovation Center for Food Nutrition and Human Health [20182008]
- Zhejiang Provincial Natural Science Foundation of China [LQ13C200006]
- program for the Science and Technology plan of Zhejiang Food and Drug Administration [SP2018031]
- Social Development Program of Hangzhou Science and Technology Committee [20180533B19]
- Zhejiang Province [2018C02053, 2017C02033]
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This study established a rapid and reliable method to determine chloramphenicol (CAP), thiamphenicol (TAP) and florfenicol (FF) residues in Chinese gelatin medicines. CAP, TAP and FF were extracted from medicine samples using 2% (v/v) ammonium hydroxide in acetonitrile. Trypsin was used to eliminate the matrix effect caused by protein components in gelatin medicines, whereas anhydrous sodium sulfate, C-18-N and NH2-PSA adsorbents were applied to reduce matrix effect induced by other components. The analytical method of these drugs was optimized on ultra high-performance liquid chromatography-mass spectrometer (UHPLC-MS/MS) through the analysis of their standard linearity and regression. The optimized extraction and analytical method were validated in one Chinese gelatin medicine sample (Colla corii asini, E Jiao) with three fortification levels (2, 5 and 10 mu g/kg), and the recoveries of these drug residues ranged of 87.6-102.7%. The limit of detection and quantification of CAP, TAP and FF in the sample were 0.2 and 0.5 mu g/kg, 0.4 and 1.5 mu g/kg, and 0.5 and 1.5 mu g/kg, respectively. A total of 30 Chinese gelatin medicine samples were analyzed using the established method. No drug residues were found in these samples except for one Testudinis Carapacis et Plastri (1.67 mu g/kg FF) and one turtle shell glue (2.55 mu g/kg FF).
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