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超高效液相色谱-串联质谱法测定鱼粉中喹噁啉类药物及其主要代谢物的残留量
其他题名Determination of quinoxalines and their major metabolites residues in fishmeal by ultra-performance liquid chromatography tandem mass spectrometry
江永远1; 王强2; 李来好2; 王旭峰2; 赵东豪2; 蔡楠2; 关婉琪2
来源期刊南方水产科学
ISSN2095-0780
出版年2019
卷号15期号:3页码:14-21
中文摘要文章建立了超高效液相色谱-串联质谱法同时检测鱼粉中5种喹噁啉类药物及其2种主要代谢物残留量的方法。样品经乙腈-乙酸乙酯(1∶1,V∶V)和1mol·L~(-1)盐酸分步提取,盐酸提取液进一步用乙酸乙酯反萃取,有机相经浓缩后,均用乙腈复溶,用PRiME HLB 通过性固相萃取柱净化处理。样品以乙腈和0.1% 甲酸水溶液为流动相,经Phenomenex Kinetex C18柱梯度洗脱分离,质谱采取正离子多反应监测模式进行检测。代谢物采用内标法定量,原药采用基质匹配外标法定量。结果表明,7种化合物在对应的浓度范围内线性关系良好(R≥0.994),2种代谢产物检测限为2mug·kg~(-1),定量限为5mug·kg~(-1);5种喹噁啉类药物检测限为1~10mug·kg~(-1);定量限为2~20mug·kg~(-1)。在高、中、低3种添加浓度下7种化合物的平均回收率为64.4%~102.2%,相对标准偏差为3.2%~10.2%。方法灵敏度高、精密度好,能同时测定鱼粉中的喹噁啉类药物及其主要代谢物。
英文摘要A sensitive and reliable ultra-high performance liquid chromatography/tandem mass spectrometry (UPLC-MS/MS) method was eatablished for the determination of olaquindox (OLA),carbadox (CBX),cyadox (CYA),quinocetone (QCT),mequindox (MEQ) and their main metabolites (QCA and MQCA) in fishmeal.The samples were extracted by acetonitrile-ethyl acetate mixture (1∶1,V∶V) and hydrochloric acid solution (1 mol·L~(-1)),then the analyte which dissolved in the aqueous phase was reextracted by ethyl acetate.The extraction was concentrated and reconstituted with acetonitrile.After purification with the Oasis PRiME HLB SPE cartridge,the sample was subjected to the following analytical procedure.The mobile phase containing acetonitrile and 0.1% formic acid solution with a linear gradient elution was utilized to separate all compounds on a Phenomenex Kinetex C18 column.The quantitative analysis of metabolites was carried out with an internal standard method and the others with an external standard method in the multiple reaction monitoring mode using positive electrospray ionization.The calibration curves for all compounds were linear (R≥0.994) within their corresponding concentration range.The recoveries were 64.4%-102.2% at different spiking levels with RSDs of 3.2%-10.2%.The limits of detection and quantification of MQCA and QCA were 2 mug·kg~(-1)and 5 mug·kg~(-1);MEQ was 10 mug·kg~(-1) and 20 mug·kg~(-1);the others were 1 mug·kg~(-1) and 2 mug·kg~(-1),respectively.This method with high sensitivity and good precision can be applied to the simultaneous determination of quinoxaline drugs and their major metabolite in fishmeal samples.
中文关键词超高效液相色谱-串联质谱法 ; 喹噁啉类药物 ; 代谢物 ; 鱼粉 ; 残留检测
英文关键词UPLC-MS/MS quinoxalines metabolites fishmeal residues determination
语种中文
国家中国
收录类别CSCD
WOS类目FOOD SCIENCE TECHNOLOGY
WOS研究方向Food Science & Technology
CSCD记录号CSCD:6507029
资源类型期刊论文
条目标识符http://119.78.100.177/qdio/handle/2XILL650/239321
作者单位1.浙江海洋大学食品与医药学院;;中国水产科学研究院南海水产研究所, ;;农业农村部水产品加工重点实验室, 舟山;;广州, 浙江;;广东 316022;;510300, 中国;
2.中国水产科学研究院南海水产研究所, 农业农村部水产品加工重点实验室, 广州, 广东 510300, 中国
推荐引用方式
GB/T 7714
江永远,王强,李来好,等. 超高效液相色谱-串联质谱法测定鱼粉中喹噁啉类药物及其主要代谢物的残留量[J],2019,15(3):14-21.
APA 江永远.,王强.,李来好.,王旭峰.,赵东豪.,...&关婉琪.(2019).超高效液相色谱-串联质谱法测定鱼粉中喹噁啉类药物及其主要代谢物的残留量.南方水产科学,15(3),14-21.
MLA 江永远,et al."超高效液相色谱-串联质谱法测定鱼粉中喹噁啉类药物及其主要代谢物的残留量".南方水产科学 15.3(2019):14-21.
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