三种常用萃取剂对罗非鱼组织中两种磺胺类药物的萃取效果比较

Compare the recovery of three reagents to sulfonamides from the tissues of GIFT nile tilapia(Oreochromis niloticus)

乙酸乙酯、乙腈和二氯甲烷是动物组织中磺胺类药物残留的常用萃取剂,但对于三者对磺胺类药物的回收效果,现有文献报道差异较大。本研究以磺胺嘧啶(SD)和磺胺间甲氧嘧啶(SMM)两种国标水产磺胺类药物为实验对象,分别在罗非鱼组织中(肌肉和血浆)加标0.5μg/g(m L),并分别使用乙酸乙酯、乙腈和二氯甲烷进行萃取,利用HPLC紫外方法检测。结果表明,乙腈萃取法的回收率最高,沉淀效果也最为理想,肌肉中SD和SMM的回收率分别为84%和87%,血浆中SD和SMM的回收率分别为88%和96%;乙酸乙酯萃取的回收率次之,分别为肌肉中78%和79%和血浆中89%和95%;二氯甲烷回收率最低,分别为肌肉中61%和67%和血浆中77%和80%。比较上述三种萃取剂的萃取结果,乙腈与乙酸乙酯萃取方法各有优劣,乙腈具有回收率高,对于血浆样品处理简便的优点,但提取液浓缩耗时较长,且毒性较大,成本较高;乙酸乙酯具有回收率高、杂质少和浓缩快速的优点;二氯甲烷回收率最低,且存在样品沉淀不完全的缺点。综合操作便捷程度及回收率,建议肌肉组织中的磺胺类药物使用10倍体积的乙酸乙酯萃取,并使用HLB固相萃取小柱进行净化;而血浆中的磺胺类药物,使用3倍体积的乙腈萃取可以达到理想的回收率。本研究比较了三种常用萃取剂对两种磺胺类药物的萃取效果,提出了适用不同样品(血浆和肌肉)的萃取方法,具有操作简便和浓缩快捷的优点。该方法适用于药物残留检测及相关研究中使用。[中国渔业质量与标准,2014,4(6):22-26]

Ethyl acetate, acetonitrile and methylene chloride were commonly used as extraction solvents to extract sulfonamides from animal tissues, but there were not consentaneous literatures for the recovery of the three agents. In this study, two sulfa drugs approved to be used in aquaculture, i. e. , sulfadiazine （SD） and sulfamonomethoxine （SMM） were acted as experimental subjects. By adding 0. 5 μg/g（mL） of sulfadiazine（SD） and sulfamonomethoxine（SMM） to the plasma and muscle of GIFT nile tilapia （ Oreochromis niloticus）. After extraction respectively by three kinds of extraction solvent and purification, HPLC ultraviolet detection method was used to detect the concentration. Results showed that the recovery when using acetonitrile was the highest, the recoveries of SD and SMM were 84% and 87% in muscle, 88% and 96% in plasma, respectively. The recoveries of ethyl acetate took the second place, which were 78% and 79% in muscles, 89% and 95% in plasma, respectively. While the recoveries of methylene chloride were not so well, the recoveries were 61% and 67% in muscles, 77% and 80% in plasma, respectively. Comparing the extraction effect of three agents, we found acetonitrile arid ethyl acetate had better recovery. Extraction method by acetonitrile had high recovery and was convenient for plasma, but it took more time for the extract concentration with higher toxicity and cost. While ethyl acetate method had higher recovery, purity, and rapid extract concentration. Re- coveries of methylene chloride were the lowest, and it could not deposit samples completely. For convenience and in- creasing recovery, we suggest that ten times the volume of ethyl acetate is used to extract the sulfonamides from muscle samples, and then purify with HLB extraction cartridges, while three times the volume of acetonitrile to extract sulfon- amides from plasma. Both can obtain ideal results. This research compared the extraction efficiency of two sulfona- mides extracted by three common extracting agents, and proposed efficient and effective extraction methods for differ- ent tissues such as muscle and plasma. These methods are applicable to the detection of drug residues and related re- searches. [ Chinese Fishery Quality and Standards, 2014, 4 （6） ：22 -26 ]