扫一扫 加微信
首页 > 期刊论文 > 论文摘要
Sin-QuEChERS净化-超高效液相色谱-串联质谱法测定鱼肉中8种喹诺酮类药物残留量
          
Determination of 8 Quinolone Drugs in Fish with Sin-QuEChERS Purification

摘    要
将粉碎后的鱼肉样品2.00 g置于50 mL离心管中,加入100 μg·L-1内标溶液200 μL和水5 mL,涡旋1 min后,用含5%(体积分数)乙酸的乙腈溶液10 mL超声提取10 min,加盐包(6 g无水硫酸镁、1.5 g氯化钠)使水相和乙腈相进行分层。涡旋、离心后,使用Sin-QuEChERS快速滤过柱直接插入离心管内,待提取液透过净化层上升至净化柱内时,移取5 mL提取液置于15 mL离心管内,加入体积比1:1的乙腈-正己烷混合液5 mL,混匀静置,取上层正己烷层涡旋,离心,于40℃氮气吹至近干,用0.2%(体积分数)甲酸溶液定容至1 mL,过滤后上机UHPLC-MS/MS,在多反应监测模式下测定8种喹诺酮类药物的残留量。结果显示:该净化方法溶剂消耗降低至10 mL,前处理时间缩短至20~25 min。环丙沙星、培氟沙星、诺氟沙星、二氟沙星和达氟沙星标准曲线的线性范围均为1.00~500.0 μg·L-1,检出限(3S/N)均为1.0 μg·kg-1;氧氟沙星、恩诺沙星和沙拉沙星标准曲线的线性范围为0.50~500.0 μg·L-1,检出限(3S/N)均为0.5 μg·kg-1。用此法平行测定同一样品7次,测定值的相对标准偏差为1.3%~6.3%。按标准加入法进行回收试验,回收率为92.0%~108%。此法用于抽检兰州4家超市的3种鱼类,8种喹诺酮类药物均未检出,说明兰州市的鱼类食品中的药物残留问题相对安全。同时,与国家农业部1077号公告-1-2008中方法进行比对,测定结果基本一致。
标    签 超高效液相色谱-串联质谱法   Sin-QuEChERS   喹诺酮   酸化乙腈   净化层   UHPLC-MS/MS   Sin-QuEChERS   quinolone   acidation acetonitrile   purifying layer  
 
Abstract
The crushed fish sample (2.00 g) was placed in a 50 mL-centrifuge tube, and 200 μL of 100 μg·L-1 internal standard solution and 5 mL of water were added. After vortex for 1 min, the above mixture was extracted ultrasonically for 10 min with 10 mL of acetonitrile solution containing 5% (φ) acetic acid, and the salts (6 g of anhydrous magnesium sulfate and 1.5 g of sodium chloride) were added to separate the aqueous phase and acetonitrile phase. After vortex and centrifugation, Sin-QuEChERS rapid filtration column was directly inserted into the centrifuge tube. When the extract rose to the purifying column through the purifying layer, 5 mL of the extract was transferred into a 15 mL-centrifuge tube, a mixture of acetonitrile and n-hexane at the volume ratio of 1:1 was added, and then the mixture was mixed well and settled. The upper n-hexane layer of was taken, then swirl, centrifuged and blown to nearly dry at 40℃ with nitrogen. The residue was made its volume to 1 mL with 0.2% (φ) formic acid solution. After filtration, 8 quinolones residues were determined by ultra high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) under multi-reaction monitoring mode. As shown by the results, the consumption of the solvent was reduced to 10 mL and the pretreatment time was shortened to 20-25 min by this purification method. The linear ranges of the standard curves of ciprofloxacin, pefloxacin, norfloxacin, difloxacin and danofloxacin were 1.00-500.0 μg·L-1, with the same detection limits (3S/N) of 1.0 μg·kg-1. The linear ranges of the standard curves of ofloxacin, enrofloxacin and sarafloxacin were 0.50-500.0 μg·L-1, with the same detection limits (3S/N) of 0.5 μg·kg-1. The same sample was determined 7 times in parallel by this method, with RSDs of the determined values in the range of 1.3%-6.3%. Test for recovery was made by standard addition method, giving results in the range of 92.0%-108%. This method was applied for sampling inspection of 3 kinds of fish from 4 supermarkets in Lanzhou, and 8 quinolones were not detected, showing that drug residues in fish food in Lanzhou were relatively safe. At the same time, the results were basically consistent with those of the method in Proclamation No. 1077-1-2008 of the State Ministry of Agriculture.

中图分类号 O657.63   DOI 10.11973/lhjy-hx202203010

 
  中国光学期刊网论文下载说明


所属栏目 工作简报

基金项目 甘肃省科技计划资助项目(20JR5RA380)

收稿日期 2020/12/23

修改稿日期

网络出版日期

作者单位点击查看


备注杨贤丰,硕士研究生,研究方向为食品安全检测

引用该论文: YANG Xianfeng,WANG Bo,ZHANG Huan,LEI Chunni,WANG Juan,LIU Ajing,XIE Yingshuang. Determination of 8 Quinolone Drugs in Fish with Sin-QuEChERS Purification[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2022, 58(3): 304~311
杨贤丰,王波,张欢,雷春妮,王娟,刘阿静,解迎双. Sin-QuEChERS净化-超高效液相色谱-串联质谱法测定鱼肉中8种喹诺酮类药物残留量[J]. 理化检验-化学分册, 2022, 58(3): 304~311


论文评价
共有人对该论文发表了看法,其中:
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
分享论文
分享到新浪微博 分享到腾讯微博 分享到人人网 分享到 Google Reader 分享到百度搜藏分享到Twitter

参考文献
【1】曹骞,代立勤,张晓伟,等.超高效液相色谱-串联质谱法检测鸡蛋中8种喹诺酮类药物残留研究[J].现代农业科技, 2019(22):183-184.
 
【2】王春,袁文峰,顾传坤,等.超高效液相色谱-三重四极杆/复合线性离子阱质谱法测定血液中11种喹诺酮类药物残留[J].分析化学, 2019,47(11):1832-1845.
 
【3】陈莉,贾春虹,刘冰洁,等.高效液相色谱-荧光检测同时测定污泥中7种氟喹诺酮类抗生素[J].地学前缘, 2019(6):7-12.
 
【4】刘承友,刘晓雷,赵兴茹,等.超声提取-超高效液相串联质谱分析沉积物中15种抗生素[J].分析试验室, 2020,39(4):410-415.
 
【5】MAURER C K, STEINBACH A, HARTMANN R W. Development and validation of a UHPLC-MS/MS procedure for quantification of the Pseudomonas quinolone signal in bacterial culture after acetylation for characterization of new quorum sensing inhibitors[J]. Journal of Pharmaceutical and Biomedical Analysis, 2013,86:127-134.
 
【6】黄瑾.LC-MS/MS法同时测定化妆品中诺氟沙星等12种喹诺酮类禁用物质[J].广东化工, 2019,46(19):241-243.
 
【7】廖华勇,王景,李红玉.超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速分析化妆品中17种喹诺酮类药物[J].分析测试学报, 2019,38(9):1102-1107.
 
【8】OVIAÑO M, RODRÍGUEZ-MARTÍNEZ J M, PASCUAL Á, et al. Rapid detection of the plasmid-mediated quinolone resistance determinant AAC(6')-Ib-cr in Enterobacteriaceae by MALDI-TOF MS analysis[J]. Journal of Antimicrobial Chemotherapy, 2017:dkw552.
 
【9】孙晓,王涛,王永姣,等.超高效液相色谱-质谱串联法测定蜂蜜中喹诺酮类药物残留[J].食品安全质量检测学报, 2019,10(17):5604-5608.
 
【10】国家质量监督检验检疫总局.动物源性食品中14种喹诺酮药物残留检测方法液相色谱-质谱/质谱法:GB/T 21312-2007[S].北京:中国标准出版社, 2008.
 
【11】王晓利,郭涛,苑金鹏,等.高效液相色谱-串联质谱法测定蔬菜中喹诺酮类抗生素残留[J].分析试验室, 2019,38(8):916-920.
 
【12】程志,宿书芳,魏莉莉,等.通过式固相萃取净化-液相色谱-串联质谱法测定豆芽中10种喹诺酮类抗生素[J].分析试验室, 2020,39(2):131-136.
 
【13】宋晓婉,梁先龙,冯娟,等.QuEChERS方法检测动物源性食品中15种喹诺酮类药物残留量及风险监测研究[J].食品安全导刊, 2019(18):89-91.
 
【14】卢剑,寻知庆,汪晨霞,等.高效液相色谱串联质谱法测定化妆品中15种喹诺酮类抗生素[J].日用化学工业, 2019,49(6):403-409.
 
【15】史艳艳,高琳,李俊,等.液相色谱-串联质谱法检测饲料中洛美沙星、培氟沙星、氧氟沙星、诺氟沙星残留[J].食品安全质量检测学报, 2019,10(11):3367-3375.
 
【16】焦慧泽,陆世清,侯迪,等.加速溶剂萃取-超高效液相色谱-串联质谱法测定茶叶中拟除虫菊酯类农药残留[J].色谱, 2019,37(6):605-611.
 
【17】钱卓真,汤水粉,梁焱,等.QuEChERS-高效液相色谱-串联质谱法同时测定水产养殖环境沉积物中磺胺类、喹诺酮类、大环内酯类抗生素[J].质谱学报, 2019,40(4):356-368.
 
【18】PASCHOAL J A R, REYES F G R, RATH S. Determination of quinolone residues in tilapias (Orechromis niloticus) by HPLC-FLD and LC-MS/MS QToF[J]. Food Additives & Contaminants:Part A, 2009,26(10):1331-1340.
 
【19】BRAGA P A D C, EBERLIN M N, REYES F G R. Applicability of MALDI-TOF MS for determination of quinolone residues in fish[J]. Journal of Mass Spectrometry, 2019,54(12):1008-1012.
 
【20】董昕.UPLC-MS/MS法同时测定动物油脂中11种喹诺酮类兽药残留[J].上海计量测试, 2019,46(4):22-25.
 
【21】权丹.牛可食性组织25种喹诺酮类药物LC-MS/MS检测方法研究[D].广州:华南农业大学, 2016.
 
【22】DORIVAL-GARCÍA N, JUNZA A, ZAFRA-GÓMEZ A, et al. Simultaneous determination of quinolone and β-lactam residues in raw cow milk samples using ultrasound-assisted extraction and dispersive-SPE prior to UHPLC-MS/MS analysis[J]. Food Control, 2016,60:382-393.
 
【23】吴学贵,王一晨,陈少莉,等.超高效液相色谱-串联质谱法同时测定罗非鱼养殖淡水中的9种喹诺酮类药物含量[J].食品安全质量检测学报, 2019,10(19):6561-6567.
 
【24】OYAMA T, NEGISHI E, ONIGAHARA H, et al. Design and synthesis of a novel pre-column derivatization reagent with a 6-methoxy-4-quinolone moiety for fluorescence and tandem mass spectrometric detection and its application to chiral amino acid analysis[J]. Journal of Pharmaceutical and Biomedical Analysis, 2015,116:71-79.
 
【25】方灵,韦航,黄彪,等.超高效液相色谱-串联质谱法同时测定牛奶中38种抗生素残留[J].分析测试学报, 2019,38(6):681-686.
 
【26】刘正才,杨方,余孔捷,等.超高效液相色谱-串联质谱法快速检测鳗鱼中磺胺类、喹诺酮类、四环素族抗生素药物残留[J].食品科学, 2009,30(14):167-170.
 
相关信息
   标题 相关频次
 超高效液相色谱指纹图谱结合化学模式识别在狼牙蜜质量评价中的应用
 6
 基于氨基酸成分分析与化学计量学的当归品质评价
 6
 超高效液相色谱-串联质谱法测定动物组织中19种兽药残留量
 4
 固相萃取-超高效液相色谱-串联质谱法测定水产品中多种兽药的残留量
 3
 Al-5Ti-1B细化剂添加量对含铈铸造铝合金组织和拉伸性能的影响
 2
 B10铜镍合金与Tup紫铜的电偶腐蚀及电绝缘
 2
 Ni-W-P-SiC脉冲复合镀层的抗高温氧化性能
 2
 QuEChERS-超高效液相色谱-串联质谱法测定血液中4种乌头类生物碱
 2
 QuEChERS净化-超高效液相色谱-串联质谱法测定番茄中5种链格孢霉毒素的含量
 2
 QuEChERS净化-超高效液相色谱-串联质谱法测定复合调味料中的爱德万甜含量
 2
 QuEChERS净化-超高效液相色谱-串联质谱法测定柑橘中7种保鲜剂的残留量
 2
 QuEChERS前处理结合超高液相色谱-串联质谱法测定高硫蔬菜中16种氨基甲酸酯类农药残留
 2
 SiCp/Al复合材料表面化学镀镍磷合金层的工艺改进
 2
 X射线衍射法定量分析蓝晶石样品
 2
 采用不含氮原料制备脱β层梯度硬质合金的组织和成分
 2
 常闭式触发开关失效分析及预防措施
 2
 超高效液相色谱-串联质谱法测定3种常见淋洗类化妆品中2种防腐剂
 2
 超高效液相色谱-串联质谱法测定茶叶中百草枯
 2
 超高效液相色谱-串联质谱法测定茶叶中印楝素A和B的残留量
 2
 超高效液相色谱-串联质谱法测定大米中34种有机含磷农药残留量
 2
 超高效液相色谱-串联质谱法测定动物源性食品中4种硝基呋喃类代谢物
 2
 超高效液相色谱-串联质谱法测定豆芽中恩诺沙星和环丙沙星
 2
 超高效液相色谱-串联质谱法测定发泡聚苯乙烯材料中的六溴环十二烷
 2
 超高效液相色谱-串联质谱法测定纺织品中致癌性染料
 2
 超高效液相色谱-串联质谱法测定蜂蜜中甲硝唑
 2
 超高效液相色谱-串联质谱法测定根痛平胶囊及片剂中松香酸和11-羰基-β-乙酰乳香酸的含量
 2
 超高效液相色谱-串联质谱法测定化妆品中21种抗组胺类药物
 2
 超高效液相色谱-串联质谱法测定化妆品中的丙烯酰胺残留
 2
 超高效液相色谱-串联质谱法测定火麻食品中特征大麻酚
 2
 超高效液相色谱-串联质谱法测定减肥保健食品中10种减肥类化合物的含量
 2