全自动固相萃取仪高浓度氯霉素样品残留清洗程序的研究  

The Study of Cleaning Procedures for Automated Solid Phase Extraction Contaminated by Samples Which Containing High Concentrations of Chloramphenicol

作　　者：肖健 谢承恩[1] 洪海燕 Xiao Jian;Xie Chengen;Hong Haiyan(Guangzhou Yuexiu Center for Disease Control and Prevention,Guangzhou 510055,China)

机构地区：[1]广州市越秀区疾病预防控制中心,广东广州510055

出　　处：《广东化工》2023年第4期23-25,共3页Guangdong Chemical Industry

基　　金：越秀区科技计划项目(2019-WS-011)。

摘　　要：本研究建立了一种适用于全自动固相萃取仪的高浓度氯霉素样本残留清洗程序。用高浓度氯霉素样本提取液上机进行固相萃取,分别用甲醇和水对进样通道、注射泵和柱塞杆三个部位进行不同体积的清洗,然后对不同清洗方法的氯霉素残留量测定结果用t检验、方差分析、SNK-q检验进行数据分析,得出最优溶剂和清洗程序。结果表明,水作为清洗溶剂清洗效果比甲醇好,Fotector-02HT全自动固相萃取仪的主要残留部位为进样通道,当样品氯霉素含量为5000μg/kg时,依次使用15 mL水和10 mL甲醇清洗进样通道,10 mL水和10 mL甲醇清洗注射泵,10 mL水和10 mL甲醇清洗柱塞杆,氯霉素残留量为0.0771μg/kg,低于方法 0.1μg/kg的检出限。该清洗程序清洗效果稳定,氯霉素残留量低,可满足高浓度氯霉素样品的残留清洗要求。To establish a cleaning procedures for automated solid phase extraction contaminated by samples which containing high concentrations of chloramphenicol. The extract solution of samples which containing high concentrations of chloramphenicol was solid phase extracted on instrument, then washed injection channel, syringe pump and plunger rod by different volume of methanol and water separately. The residual concentration of chloramphenicol was detected and results were analyzed by t-test, ANOVA and SNK-q test to find out the best solvent and cleaning procedure. The cleaning effect of water is better than that of methanol. The main residual part of Fotector-02HT automated solid phase extraction was the injection channel. If a sample which contain 5000 μg/kg of chloramphenicol was solid phase extracted on instrument, washed the injection channel with 15 mL water and 10 mL methanol, washed the syringe pump with 10 mL water and 10 mL methanol and washed the plunger rod with 10 mL water and 10 mL methanol in turn can reduce the residue to 0.0771 μg/kg, which was lower than the detection limit of 0.1 μg/kg. The cleaning effect of the cleaning procedure is stable and the chloramphenicol residue was low, it can meet the residual cleaning requirements of samples which containing high concentrations of chloramphenicol.

关 键 词：全自动固相萃取仪 氯霉素 清洗程序 超高效液相色谱-串联质谱 

分 类 号：R155[医药卫生—营养与食品卫生学]