在线固相萃取/液相色谱-串联质谱法研究饲料中5种喹噁啉药物残留量检测
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- 英文论文题名：Study on Determination of 5 Quinoxalines Residue in Feed by On-line Solid Phase Extraction/Liquid Chromatography-Tandem Mass Spectrometry Method
- 论文作者：吴剑平 ; 张鑫 ; 李丹妮 ; 严凤 ; 周悦榕 ; 顾欣
- 英文论文作者：WU Jian-ping ; ZHANG Xin ; LI Dan-ni ; YAN Feng ; ZHOU Yue-rong ; GU Xin ; Shanghai Municipal Supervisory Institute of Veterinary Drugs and Feedstaff
- 年：2016
- 作者机构：上海市兽药饲料检测所;
- 论文关键词：在线固相萃取 ; 双三元液相色谱-串联质谱法 ; 喹噁啉类药物 ; 饲料
- 英文论文关键词：on-line SPE ; double ternary liquid chromatography-tandem mass spectrometry ; quinoxalines ; feed
- 会议召开时间：2016-09-18
- 会议录名称：中国畜牧兽医学会动物药品学分会第五届全国会员代表大会暨2016年学术年会论文集
- 语种：中文
- 分类号：S816.17
- 学会代码：ZGXJ
- 会议名称：中国畜牧兽医学会动物药品学分会第五届全国会员代表大会暨2016年学术年会
- 会议地点：中国四川成都
- 主办单位：中国畜牧兽医学会动物药品学分会
- 学会名称：中国畜牧兽医学会
- 页数：8
- 文件大小：1089k
- 原文格式：O
- 会议级别：全国
摘要
建立了在线固相萃取/液相色谱串联质谱法检测饲料中5种喹嗯啉药物的方法。准确称取2g饲料,用10mL0.1%盐酸-甲醇(1:1)提取,提取液用0.2%甲酸稀释10倍,通过双三元液相色谱用反相在线同相萃取柱在线富集净化,以0.2%甲酸与乙腈梯度洗脱,同时转移至C18色谱柱上进行分离,串联四极杆质谱检测。实验结果表明,5种喹嗯啉药物在50~25000μg/kg含量范围内线性良好(r≥0.999);方法的检出限为25μg/kg,定量下限为50μg/kg;方法回收率为70%~90%,批内和批间相对标准偏差均小于10%。本方法较传统固相萃取柱净化法更简捷、经济和稳定。
A high performance liquid chromatography-tandem mass spectrometry method with on-line SPE(solid phase extraction) was established for determination of 5 quinoxaline residues in feed.2g feed was extracted with 10 mL 0.1%HCl-CH_3OH(1:1).The extraction was 10 times diluted by 0.2%formic acid.The dissolution was enriched and purified by the reverse phase on-line SPE column on a double ternary liquid chromatography.Target compounds were eluted with 0.2%formic acid and acetonitrile in gradient mode and separated with an octadecyl silica bonded column.Target compounds was then determined by the tandem mass spectrometry.The results showed that the linearity of 5 quinoxalines was good in the range of 50-25000 μg/kg(r≥0.999).The LOD of the method was 25 μg/kg,while the LOQ was 50 μg/kg.Recoveries of the 5 quinoxalines were in the range of 70%-90%,while the RSD of both in the batch and between the batch were all lower than 10%.The method was proved to be more convenient,economical and stable than the traditional column-SPE method.
A high performance liquid chromatography-tandem mass spectrometry method with on-line SPE(solid phase extraction) was established for determination of 5 quinoxaline residues in feed.2g feed was extracted with 10 mL 0.1%HCl-CH_3OH(1:1).The extraction was 10 times diluted by 0.2%formic acid.The dissolution was enriched and purified by the reverse phase on-line SPE column on a double ternary liquid chromatography.Target compounds were eluted with 0.2%formic acid and acetonitrile in gradient mode and separated with an octadecyl silica bonded column.Target compounds was then determined by the tandem mass spectrometry.The results showed that the linearity of 5 quinoxalines was good in the range of 50-25000 μg/kg(r≥0.999).The LOD of the method was 25 μg/kg,while the LOQ was 50 μg/kg.Recoveries of the 5 quinoxalines were in the range of 70%-90%,while the RSD of both in the batch and between the batch were all lower than 10%.The method was proved to be more convenient,economical and stable than the traditional column-SPE method.
引文
[1]苑鹤,王卫娜,吴秋华,王春,王志.磁性石墨烯固相萃取原子吸收法测定环境水样中的痕量铜[J].分析测试学报,2013,32(1):69-73.
[2]李婷,汤智,洪武兴.分散固相萃取气相色谱质谱法测定含油脂食品中17种邻苯二甲酸酯[J].分析化学,2012,40(3):391-396.
[3]尹怡,郑光明,朱新平,马丽莎,吴仕辉,潘德博,戴晓欣,谢文平.分散固相萃取气相色谱质谱联用快速测定鱼虾中的16种多环芳烃[J].分析测试学报,2013,30(10):1107-1112.
[4]Zhao L,Kestell P,Philipott M,Ching L M,Zhuang L,Baguley B C.The antitumour activity of5,6-dimethylxanthenone-4-acetic acid(DMXAA)in TNF receptor-1 knockout mice[J].Cancer Chemother.Pharmacol,2001,47(3):491-497.
[5]吴剑平,张鑫,顾欣,李丹妮,严凤,周悦榕.分散液相微萃取/超高效液相色谱-串联质谱法检测猪尿中盐酸赛庚啶残留量的研究[J].分析测试学报,2013,32(7):834-839.
[6]Lee H B,Peart T E,Svoboda M L.Determination of ofloxacin,norfloxacin,and ciprofloxacin in sewage by selective solid-phase extraction,liquid chromatography with fluorescence detection,and liquid chromatography—tandem mass spectrometry[J].J.Chromatogr.A,2007,1139(1):45-52.
[7]Yang Y,Shao B,Zhang J.Determination of the residues of 50 anabolic hormones in muscle,milk and liver by very-high-pressure liquid chromatography-electrospray ionization tandem mass spectrometry[J].J.Chromatogr.B,2009,877(5/6):489.
[8]艾连峰,马育松,陈瑞春,郭春海,康占省.在线净化液相色谱串联质谱法测定动物源食品中金刚烷胺的残留[J].分析化学,2013,41(8):1194-1198.
[9]Mottier P,Hammel Y A,Gremaud E,Guy P A.Quantitative High-Throughput Analysis of 16(Fluoro)quinolones in Honey Using Automated Extraction by Turbulent Flow Chromatography Coupled to Liquid Chromatography-Tandem Mass Spectrometry[J].J.Agric.Food Chem.,2008,56(1):35-43.
[10]Roach J A G,Dibussolo J M,Krynitsky A,Noonan G O.Evaluation and single laboratory validation of an on-line turbulent flow extraction tandem mass spectrometry method for melamine in infant forrnula[J].J.Chromatogr.A,2011,1218(1):4284-4290.
[11]黄雄风,刘召金,陈静,戴振宇,许群,庄国顺.超高效液相色谱法检测猪肉中乙酰甲喹及其主要代谢物[J].分析测试学报,2014,33(1):39-44.
[12]杨盼盼.喹嗯啉类遗传毒性分子机制[D].武汉:华中农业大学,2013.
[13]赵春保,彭大鹏,陶燕飞,陈冬梅,袁宗辉.猪饲料中喹噁啉类药物酶联免疫检测方法的建立[J].中国农业科技导报,2008,10(S2):69-53.
[14]利光辉,杨帆,林燕茹,方其丰.超高效液相色谱法检测猪肉中乙酰甲喹及其主要代谢物[J].动物医学进展,2013,34(1):38-42。
[15]赵珊,郭巧珍,张晶,邵兵.超高压液相色谱_串联质谱法测定鱼组织中卡巴氧及喹乙醇代谢物[J].食品安全质量检测学报,2013,4(1):124-128.
[2]李婷,汤智,洪武兴.分散固相萃取气相色谱质谱法测定含油脂食品中17种邻苯二甲酸酯[J].分析化学,2012,40(3):391-396.
[3]尹怡,郑光明,朱新平,马丽莎,吴仕辉,潘德博,戴晓欣,谢文平.分散固相萃取气相色谱质谱联用快速测定鱼虾中的16种多环芳烃[J].分析测试学报,2013,30(10):1107-1112.
[4]Zhao L,Kestell P,Philipott M,Ching L M,Zhuang L,Baguley B C.The antitumour activity of5,6-dimethylxanthenone-4-acetic acid(DMXAA)in TNF receptor-1 knockout mice[J].Cancer Chemother.Pharmacol,2001,47(3):491-497.
[5]吴剑平,张鑫,顾欣,李丹妮,严凤,周悦榕.分散液相微萃取/超高效液相色谱-串联质谱法检测猪尿中盐酸赛庚啶残留量的研究[J].分析测试学报,2013,32(7):834-839.
[6]Lee H B,Peart T E,Svoboda M L.Determination of ofloxacin,norfloxacin,and ciprofloxacin in sewage by selective solid-phase extraction,liquid chromatography with fluorescence detection,and liquid chromatography—tandem mass spectrometry[J].J.Chromatogr.A,2007,1139(1):45-52.
[7]Yang Y,Shao B,Zhang J.Determination of the residues of 50 anabolic hormones in muscle,milk and liver by very-high-pressure liquid chromatography-electrospray ionization tandem mass spectrometry[J].J.Chromatogr.B,2009,877(5/6):489.
[8]艾连峰,马育松,陈瑞春,郭春海,康占省.在线净化液相色谱串联质谱法测定动物源食品中金刚烷胺的残留[J].分析化学,2013,41(8):1194-1198.
[9]Mottier P,Hammel Y A,Gremaud E,Guy P A.Quantitative High-Throughput Analysis of 16(Fluoro)quinolones in Honey Using Automated Extraction by Turbulent Flow Chromatography Coupled to Liquid Chromatography-Tandem Mass Spectrometry[J].J.Agric.Food Chem.,2008,56(1):35-43.
[10]Roach J A G,Dibussolo J M,Krynitsky A,Noonan G O.Evaluation and single laboratory validation of an on-line turbulent flow extraction tandem mass spectrometry method for melamine in infant forrnula[J].J.Chromatogr.A,2011,1218(1):4284-4290.
[11]黄雄风,刘召金,陈静,戴振宇,许群,庄国顺.超高效液相色谱法检测猪肉中乙酰甲喹及其主要代谢物[J].分析测试学报,2014,33(1):39-44.
[12]杨盼盼.喹嗯啉类遗传毒性分子机制[D].武汉:华中农业大学,2013.
[13]赵春保,彭大鹏,陶燕飞,陈冬梅,袁宗辉.猪饲料中喹噁啉类药物酶联免疫检测方法的建立[J].中国农业科技导报,2008,10(S2):69-53.
[14]利光辉,杨帆,林燕茹,方其丰.超高效液相色谱法检测猪肉中乙酰甲喹及其主要代谢物[J].动物医学进展,2013,34(1):38-42。
[15]赵珊,郭巧珍,张晶,邵兵.超高压液相色谱_串联质谱法测定鱼组织中卡巴氧及喹乙醇代谢物[J].食品安全质量检测学报,2013,4(1):124-128.