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, C18-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 μg/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 μg/kg, 0.4 and 1.5 μg/kg, and 0.5 and 1.5 μg/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 μg/kg FF) and one turtle shell glue (2.55 μg/kg FF).

中文翻译：

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分散固相萃取-超高效液相色谱-质谱法测定中药明胶中的氯霉素，甲砜霉素和氟苯尼考

这项研究建立了一种快速可靠的方法来测定明胶药物中的氯霉素（CAP），甲砜霉素（TAP）和氟苯尼考（FF）残留量。使用乙腈中的2％（v / v）氢氧化铵从药物样品中提取CAP，TAP和FF。胰蛋白酶用于消除明胶药物中蛋白质成分引起的基质效应，而无水硫酸钠，C18-N和NH2-PSA吸附剂则用于降低其他成分引起的基质效应。通过分析其标准线性和回归，在超高效液相色谱-质谱仪（UHPLC-MS / MS）上优化了这些药物的分析方法。在一种具有三个设防水平的中药样品（Colla corii asini，E Jiao）中验证了优化的提取和分析方法。5和10μg/ kg），这些药物残留的回收率范围为87.6-102.7％。样品中CAP，TAP和FF的检出限和定量限分别为0.2和0.5μg/ kg，0.4和1.5μg/ kg，0.5和1.5μg/ kg。使用建立的方法对总共30种明胶药品样品进行了分析。除了一种Testudinis Carapacis et Plastri（1.67μg/ kg FF）和一种乌龟壳胶（2.55μg/ kg FF），在这些样品中未发现药物残留。