干旱区生态环境知识资源中心(Arid): 畜禽粪便和污水中金霉素及其代谢物的液质联用(LC-MS/MS)检测方法研究

Arid

	畜禽粪便和污水中金霉素及其代谢物的液质联用(LC-MS/MS)检测方法研究
其他题名	An innovated analytical method for determine the CTC and its metabolites in animal excreta and sewage by LC - MS/MS
	王冉 1; 魏瑞成 1; 葛峰 2; 裴燕 1; 冯国兴 1; 王恬 3
来源期刊	安全与环境学报
ISSN	1009-6094
出版年	2011
卷号	11 期号:3 页码:115-118
中文摘要	建立了畜禽粪便和污水中金霉素(CTC)及其两种代谢物差向金霉素(ECTC)和异金霉素(ICTC)的LC-MS/MS检测方法。粪便样品经Na2EDTA-McIlvaine缓冲液(pH=4)分别提取3次,离心,收集上清液,过Waters的Oasis HLB固相萃取小柱净化、浓缩。用6 mL 0.01 mol·L~(-1)草酸甲醇溶液洗脱,收集洗脱液,40 ℃水浴氮气吹至近干,甲醇定容至1 mL,过0.22 mum滤膜,用LC-MS/MS测定。污水取100 mL经滤纸和0.65 mum纤维膜过滤后,加1 mL 5% Na2EDTA溶液,调节pH值至7.0,然后过预先用5 mL甲醇和10 mL Na2EDTA-McIlvaine缓冲液(pH=4)活化过的Waters Oasis HLB固相萃取小柱,净化、浓缩,后用6 mL 0.01 mol·L~(-1)草酸甲醇溶液洗脱,收集洗脱液,40 ℃水浴氮气吹至近干,甲醇定容至1 mL,过0.22 mum滤膜,上机测定。该方法在10~1 000 mug·L~(-1)之间呈线性相关,金霉素、差向金霉素和异金霉素的平均回收率分别为79.64%~97.23%、75.34%~98.37%和73.67%~95.08%,日间偏差在1.78%~6.18%,日内偏差在1.07%~6.28%。粪便样品和污水样品中的检测限分别为20 mug·kg~(-1)和10 mug·L~(-1),符合作为检测方法的要求。
英文摘要	This paper aims to introduce a sensitive LC-MS/MS analytical method for determining CTC,ECTC and ICTC in animal excreta and sewage developed by the present author.As we know,for the time being,the most frequently used antibacterial for treating animal disease and young animal growth-promotor is Chlortetracycline (CTC).However,CTC cann’t be fully absorbed and a considerable amount of CTC and its main metabolites were excreted directly into the excreta in reality.For this reason,it has become a great concern for the potential risk of the manure-derived CTC and its main metabolites that may permeate into the surface water.In order to find effective resistant microorganism to deal with the problem,we have done experiments by extracting animal excreta samples three times by using 6 mL 0.1 mol·L~(-1)Na2EDTA-Mcllvaine buffer (pH=4)and then cleaned the samples up by using Oasis HLB solid phase extraction (SPE)column.Later,the sewage was let to be filtrated by 0.65 mum film firstly and then mixed with 5% Na2EDTA.In doing so,the solution was then treated on the Oasis HLB column after their pH value was adjusted to 7.The analytes were then separated by means of liquid chromatography and determined with liquid chromatography coupled to tandem mass spectrometry under the electro-sprayed ion and multiple reaction monitor mode.The results indicate that the calibration curves for CTC,ECTC and ICTC turned to be linear at a concentration range of 0.01-1.0 mg·L~(-1),with the correlation coefficients being from 0.998 7 to 0.999 7,respectively.The limits of detection (LOD)for CTC,ECTC and ICTC prove to be 20 mug·kg~(-1)in animal excretion and 10 mug·L~(-1)in the sewage.The average recovery rate of CTC,ECTC and ICTC spiked samples was made to reach 79.64%-88.73%,75.34%-87.34% and 73.67-84.21% in animal excretion,respectively,and 93.27%-97.23%,91.34%-98.37% and 93.15%-95.08% in the sewage.The inter-day standard deviations (RSD)and intra-day RSD deviations tend to range from 1.78% to 6.18% and from 1.07% to 6.28%,respectively.Thus,that the method developed in this study is simple in operation,sensitive and repeatable,as well as favorable for the simultaneous determination of CTC,ECTC and ICTC either in animal excretion or in the sewage.
中文关键词	畜牧 ; 兽医科学其他学科 ; 畜禽粪便 ; 污水 ; 金霉素 ; 差向金霉素 ; 异金霉素 ; 液质联用法
英文关键词	other disciplines of animal husbandry and veterinary medicines animal excrement wastewater CTC ECTC ICTC LC- MS/MS
语种	中文
国家	中国
收录类别	CSCD
WOS类目	ENVIRONMENTAL SCIENCES
WOS研究方向	Environmental Sciences & Ecology
CSCD记录号	CSCD:4300571
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/226151
作者单位	1.江苏省农业科学院, 农业部食品安全监控重点开放实验室;;江苏省畜禽产品安全性研究重点实验室, 南京, 江苏 210014, 中国; 2.环境保护部南京环境科学研究所, 南京, 江苏 210012, 中国; 3.南京农业大学动物科技学院, 南京, 江苏 210095, 中国
推荐引用方式 GB/T 7714	王冉,魏瑞成,葛峰,等. 畜禽粪便和污水中金霉素及其代谢物的液质联用(LC-MS/MS)检测方法研究[J],2011,11(3):115-118.
APA	王冉,魏瑞成,葛峰,裴燕,冯国兴,&王恬.(2011).畜禽粪便和污水中金霉素及其代谢物的液质联用(LC-MS/MS)检测方法研究.安全与环境学报,11(3),115-118.
MLA	王冉,et al."畜禽粪便和污水中金霉素及其代谢物的液质联用(LC-MS/MS)检测方法研究".安全与环境学报 11.3(2011):115-118.