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蜂蜜中14种喹诺酮类药物残留的高效液相色谱-串联质谱测定
其他题名Simultaneous Determination of 14 Quinolones Residues in Honey by High Performance Liquid Chromatography- Tandem Mass Spectrometry
曹彦忠1; 庞国芳1; 张进杰1; 石玉秋1; 李学民1; 范春林1; 刘永明1; 贾光群1; 刘晓茂1; 张艳梅2
ISSN1004-4957
出版年2008
卷号27期号:11页码:1141-1146
中文摘要建立了同时测定蜂蜜中14种喹诺酮类药物残留的高效液相色谱-串联质谱分析方法。蜂蜜中喹诺酮类药物残留用0.05mol/L磷酸盐缓冲溶液(pH:3.0)提取,样液过滤后,经OasisHLB固相萃取柱净化,氢氧化铵-甲醇溶液(体积比1:19)洗脱,蒸干定容后,用反相液相色谱分离,电喷雾正离子模式离子化,用多反应监测方式(MRM)监测,三重四极杆质谱测定。环丙沙星在0.4~100.0mug/kg,嗯喹酸在0.4~50.0mug/kg,恩诺沙星、沙拉沙星、双氟沙星、依诺沙星、诺氟沙星在1.0~100.0mug/kg,氧氟沙星、单诺沙星、氟罗沙星、奥比沙星、麻保沙星在1.0~50.0mug/kg,司帕沙星、氟甲喹在2.0~100.0mug/kg范围内呈线性关系,相关系数r〉0.997,在2.0、5.0、10.0、50.0mug/kg4个添加水平,回收率为66%~111%,相对标准偏差(RSD)为1.3%-13.6%。该方法操作简便,稳定性好,选择性好,灵敏度高,其检出限达1.0mug/kg。
英文摘要A high performance liquid chromatography- tandem mass spectrometry (HPLC -MS/MS) method was established for simultaneous determination of 14 quinolones residues in honey. The sam- ple were extracted with 0.05 mol/L phosphate buffer solution( pH = 3.0). After filtration, the extract was purified by Oasis HLB solid phase extraction column and eluted with methanol - ammonia solution ( 19:1 ,by volume) , and then it was evaporated to dry under nitrogen and redissolved in 1 mL dissolving solution. The solution was separated on a RP-HPLC column and detected by triple-quadrupole MS. The electrospray was operated in the positive ionization mode and the quinolones were identified by using multiple reaction monitoring(MRM) mode. Linear ranges for 14 quinolones were as follows: eiprofloxacin(0.4 - 100.0 mug/kg) ; oxolinic acid(0. 4 - 50.0 mug/kg) ; enrofloxacin, sarafloxacin, difloxaein, enoxacin and norfloxaein( 1.0 -100.0 mug/kg) ; ofloxaein, danofloxacin, fleroxacin, orbi- floxacin and marbofloxacin( 1.0 - 50. 0 mug/kg) ; sparfloxacin and flumequin(2.0 - 100. 0 mug/kg). Correlation coefficients were more than 0. 997. Recoveries at the four spiked levels of 2. 0, 5.0, 10. 0 and 50. 0 mug/kg ranged from 66% - 111% , and relative standard deviations(RSDs) were in the range of 1.3% - 13.6% . The limits of detection for the method were 1.0 mug/kg. Owing the merits of sire-plicity, selectivity and sensitivity, the proposed method has been successfully applied to the determination of quinolones residues in honey.
中文关键词蜂蜜 ; 喹诺酮类药物 ; 固相萃取 ; 液相色谱-串联质谱法
英文关键词honey quinolones solid phase extraction liquid chromatography -tandem mass spec- trometry
语种中文
国家中国
收录类别CSCD
WOS类目CHEMISTRY ANALYTICAL
WOS研究方向Chemistry
CSCD记录号CSCD:3473423
资源类型期刊论文
条目标识符http://119.78.100.177/qdio/handle/2XILL650/222209
作者单位1.秦皇岛出入境检验检疫局, 秦皇岛, 河北 066002, 中国;
2.河北大学化学与环境科学学院, 保定, 河北 071002, 中国
推荐引用方式
GB/T 7714
曹彦忠,庞国芳,张进杰,等. 蜂蜜中14种喹诺酮类药物残留的高效液相色谱-串联质谱测定[J],2008,27(11):1141-1146.
APA 曹彦忠.,庞国芳.,张进杰.,石玉秋.,李学民.,...&张艳梅.(2008).蜂蜜中14种喹诺酮类药物残留的高效液相色谱-串联质谱测定.,27(11),1141-1146.
MLA 曹彦忠,et al."蜂蜜中14种喹诺酮类药物残留的高效液相色谱-串联质谱测定".27.11(2008):1141-1146.
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