搜索热:失效分析 陶瓷
扫一扫 加微信
首页 > 期刊论文 > 论文摘要
分散固相萃取-液相色谱-串联质谱法测定蜂蜜中新型烟碱类杀虫剂及其代谢物的残留量
          
Simultaneous Determination of Neonicotinoid Insecticides and Their Metabolites in Honey by High Performance Liquid Chromatography-Tandem Mass Spectrometry with Dispersive Solid-Phase Extraction

摘    要
称取蜂蜜样品2.00 g至具塞离心管中,加入100 μL同位素内标溶液(200 μg·L-1)和10 mL水,涡旋混匀,加入甲醇至20 mL,涡旋混匀,以8 500转·min-1离心5 min,移取上清液0.50 mL,用甲醇定容至10.0 mL,涡旋混匀后,以8 500转·min-1离心5 min,取1.0 mL上清液转移至具塞离心管中(内含混合均匀的吸附剂:30 mg N-丙基乙二胺、15 mg C18粉末和50 mg无水MgSO4),涡旋混匀进行吸附净化,以8 500转·min-1离心5 min,转移全部上清液,于40℃下用氮气吹至近干,用甲醇-0.15%(体积分数,下同)甲酸溶液(1+9)混合液溶解残渣并定容至1.0 mL,过0.22 μm滤膜后供液相色谱-串联质谱分析。采用Agilent Eclipse XDB-C18色谱柱进行分离,以不同比例的含5 mmol·L-1乙酸铵的0.15%甲酸溶液和甲醇为流动相进行梯度洗脱。质谱中采用电喷雾离子源正离子扫描方式和多反应监测模式,采用同位素内标法和外标法进行定量。吡蚜酮、呋虫胺、烯啶虫胺、噻虫嗪、氟啶虫酰胺、吡虫啉、噻虫胺、氯噻啉、啶虫脒、噻虫啉、4-(三氟甲基)烟酰胺和N-去甲基啶虫脒的质量浓度在一定范围内呈线性,测定下限(10S/N)在2.5~12.5 μg·kg-1之间。对空白蜂蜜样品进行加标回收试验,回收率在79.9%~108%之间,测定值的相对标准偏差(n=6)在1.7%~15%之间。
标    签 液相色谱-串联质谱法   分散固相萃取   新型烟碱类杀虫剂   蜂蜜   high performance liquid chromatography-tendam mass spectrometry   dispersive solid-phase extraction   neonicotinoid insecticide   honey  
 
Abstract
The honey sample (2.00 g) was added into in a centrifuge tube with a cover, and 100 μL of isotope internal standard solution (200 μg·L-1) and 10 mL water were added. After mixing well by vortex, the mixture was made up to 20 mL with methanol, and mixed well, centrifuged at 8 500 r·min-1 for 5 min. 0.50 mL of the supernatant was taken and diluted to 10.0 mL with methanol, and the mixture was mixed well by vortex, then centrifuged at 8 500 r·min-1 for 5 min. 1.0 mL of the supernatant was transferred into a centrifuge tube containing a homogeneously mixed adsorbent (30 mg of N-propyl ethylenediamine, 15 mg of C18 powder and 50 mg of anhydrous MgSO4). After vortexing and mixing for adsorption purification, the tube was centrifuged at 8 500 r·min-1 for 5 min. All the supernatant was blowed to near dryness using nitrogen at 40 ℃, and the residue was disolved and made up to 1.0 mL with a mixture of methanol and 0.15% (volume fraction) formic acid solution (1+9). The solution was passed through a 0.22 μm filter, and the filtrate was analyzed by liquid chromatography-tandem mass spectrometry. Chromatographic separation was carried out using an Agilent Eclipse XDB-C18 column, with a mixture in varying proportions of 0.15% formic acid solution containing 5 mmol·L-1 ammonium acetate and methanol as mobile phase for gradient elution. Electrospray ion source, positive ion scanning mode and multireaction monitoring mode were used in the mass spectrometry, and the isotope dilution internal standard method and external standard method were used for quantification. The mass concentration of pyridoxine, dinotefuran, nitenpyram, thiame-thoxam, flonicamid, imidacloprid, clothianidin, chlorothiazide, acetamiprid, thiacloprid, 4-(trifluoromethyl)nicotinamide and N-desmethylpyrazole, was linear within definite ranges, and the lower limits of determination (10S/N) were between 2.5-12.5 μg·kg-1. Tests for recovery was made by standard addition method to blank honey samples, giving results in the range of 79.9%-108%, and RSDs (n=6) were between 1.7% and 15%.

中图分类号 O657.6   DOI 10.11973/lhjy-hx201903005

 
  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 国家质检总局科技计划项目(2016IK280);浙江出入境检验检疫局科技计划项目(ZK201710X)

收稿日期 2018/5/19

修改稿日期

网络出版日期

作者单位点击查看

备注侯建波,高级工程师,博士,研究方向为食品中药物残留分析,houjb@ziq.gov.cn

引用该论文: HOU Jianbo,XIE Wen,QIAN Yan,WANG Peng,LEI Meikang,CHEN Yunyin. Simultaneous Determination of Neonicotinoid Insecticides and Their Metabolites in Honey by High Performance Liquid Chromatography-Tandem Mass Spectrometry with Dispersive Solid-Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2019, 55(3): 270~277
侯建波,谢文,钱艳,汪鹏,雷美康,陈允吟. 分散固相萃取-液相色谱-串联质谱法测定蜂蜜中新型烟碱类杀虫剂及其代谢物的残留量[J]. 理化检验-化学分册, 2019, 55(3): 270~277


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】PASTOR-BELDA M, GARRIDO I, CAMPILLO N, et al. Determination of spirocyclic tetronic/tetramic acid derivatives and neonicotinoid insecticides in fruits and vegetables by liquid chromatography and mass spectrometry after dispersive liquid-liquid microextraction[J]. Food Chemitry, 2016,202:389-395.
 
【2】CHAGNON M, KREUTZWEISER D, MITCHELL E A, et al. Risks of large scale use of systemic insecticides to ecosystem functioning and services[J]. Environmental Science and Pollution Research, 2012,22:119-134.
 
【3】LU C, WARCHOL K M, CALLAHAN R A. In situ replication of honey bee colony collapse disorder[J]. Bulletin of Insectology, 2012,65:99-106.
 
【4】LAURINO D, MANINO A, PATETTA A, et al. Toxicity of neonicotinoid insecticides on different honey bee genotypes[J]. Bulletin of Insectology, 2013,66(1):119-126.
 
【5】VICHAPONG J, BURAKHAM R, SRIJARANAI S. In-coupled syringe assisted octanol-water partition microextraction coupled with high-performance liquid chromatography for simultaneous determination of neonicotinoid insecticide residues in honey[J]. Talanta, 2015,139:21-26.
 
【6】MITCHELL E A D, MULHAUSER B, MULOT M, et al. A world wide survey of neonicotinoids in honey[J]. Science, 2017,358:109-111.
 
【7】The European Union. EU pesticides data-base[EB/OL].[2018-05-01] http://ec.europa.eu/food/plant/pesticides.
 
【8】Japan. Positive list system for agricultural chemical residues in foods[EB/OL].[2018-05-01] http://www.mhlw.go.jp/english/topics/foodsafety/positivelist060228/2018/05/01.
 
【9】许秀莹,施海燕,王鸣华.气相色谱-质谱联用测定大米中6种烟碱类农药残留[J].质谱学报, 2012,33(2):99-103.
 
【10】侯如燕,蔡荟梅,张正竹,等.液相色谱法检测水果蔬菜中的烟碱类农药残留[J].分析试验室, 2010,29(2):59-63.
 
【11】侯如燕,卞红正,赵秀霞,等.固相萃取-液相色谱测定复杂基质蔬菜中9种烟碱类残留[J].分析测试学报, 2011,30(1):58-63.
 
【12】KO A Y, RAHMAN M M, El-ATY A M A, et al. Development of a simple extraction and oxidation procedure for the residue analysis of imidacloprid and its metabolites in lettuce using gas chromatography[J]. Food Chemistry, 2014,148:402-409.
 
【13】GB/T 19648-2006水果和蔬菜中500种农药及相关化学品残留量的测定气相色谱-质谱法[S].
 
【14】GB/T 20769-2008水果和蔬菜中450种农药及相关化学品残留量的测定液相色谱-串联质谱法[S].
 
【15】GB/T 23205-2008茶叶中448种农药及相关化学品残留量的测定液相色谱-串联质谱法[S].
 
【16】GARCIA M D G, GALERA M M, VALVERDE R S, et al. Column switching liquid chromatography and post-column photochemically fluorescence detection to determine imidacloprid and 6-chloronicotinic acid in honeybees[J]. Journal of Chromatography A, 2007,1147(1):17-23.
 
【17】RANCAN M, SABATINI A G, ACHILLI G, et al. Determination of imidacloprid and metabolites by liquid chromatography with an electrochemical detector and post column photochemical reactor[J]. Analytica Chimica Acta, 2006,555:20-24.
 
【18】CAMPILLO N, VINAS P, FEREZ-MELGAREJO G, et al. Liquid chromatography with diode array detection and tandem mass spectrometry for the determination of neonicotinoid insecticides in honey samples using dispersive liquid-liquid microextraction[J]. Journal of Agricultural and Food Chemistry, 2013,61:4799-4805.
 
【19】王东,侯传金,赵尔成,等.盐析辅助均相液液萃取/分散固相萃取-超高效液相色谱串联质谱法测定蜂蜜中新烟碱类农药残留[J].分析测试学报, 2015,34(6):681-685.
 
【20】粟有志,李芳,齐鑫,等.QuEChERS-高效液相色谱/串联质谱法同时测定蜂蜜中9种新烟碱类杀虫剂残留[J].分析科学学报, 2015,31(2):203-207.
 
【21】TANNER G, CZERWENKA C. LC-MS/MS Analysis of neonicotinoid insecticides in honey methodology and residue findings in Austrian honeys[J]. Journal of Agricultural and Food Chemistry, 2011,59:12271-12277.
 
【22】JIAO W T, XIAO Y, QIAN X S, et al. Optimized combination of dilution and refined QuEChERS to overcome matrix effects of six types of tea for determination eight neonicotinoid insecticides by ultra performance liquid chromatography-electrospray tandem mass spectrometry[J]. Food Chemistry, 2016,210:26-34.
 
【23】GBYLIK-SIKORSKA M, SNIEGOCKI T, POSYNIAK A. Determination of neonicotinoid insecticides and their metabolites in honey bee and honey by liquid chromatography tandem mass spectrometry[J]. Journal of Chromatography B, 2015,990:132-140.
 
【24】SUGANTHI A, BHUVANESWARI K,RAMYA M. Determination of neonicotinoid insecticide residues in sugarcane juice using LC-MS/MS[J]. Food Chemistry, 2018,241:275-280.
 
【25】STAHNKE H, KITTLAUS S, KEMPE G N, et al. Reduction of matrix effectsin liquid chromatography-electrospray ionization-mass spectrometry by dilution of the sample extracts:How much dilution is needed?[J]. Analytical Chemistry, 2012,84(3):1474-1482.
 
相关信息
   标题 相关频次
 液相色谱-串联质谱法测定蜂蜜中双甲脒及其代谢产物残留量
 9
 固相萃取-液相色谱-串联质谱法同时测定葛根中11种黄酮苷元的含量
 7
 超高效合相色谱法拆分和测定婴幼儿配方乳粉中肉碱对映体
 6
 超高效合相色谱法快速测定婴幼儿辅食果泥中甲氰菊酯对映体的残留量
 4
 固相萃取-超高效合相色谱法测定猪肉中氟苯尼考对映体及其代谢物氟苯尼考胺的含量
 4
 牛奶中碳、氮、氢和氧稳定同位素比的测定及其在产地溯源分析中的应用
 4
 液相色谱-串联质谱法测定牛奶中11种真菌毒素残留量
 4
 液相色谱-串联质谱法测定葡萄酒中赭曲霉毒素A、B的残留量
 4
 液相色谱-串联质谱法同时测定水产品中三苯甲烷类与噻嗪类染料及其代谢产物
 4
 高效液相色谱法测定化妆品中5种荧光增白剂
 3
 高效液相色谱法测定进口葡萄酒中的白藜芦醇及其甙
 3
 液相色谱-串联质谱法测定虾肉中7种非食用色素的残留量
 3
 45圆钢冷拔加工开裂原因分析
 2
 QuEChERS净化-高效液相色谱-串联质谱法测定蜂蜜中农药及抗生素的含量
 2
 超高效液相色谱-串联质谱法测定蜂蜜中的14种杀虫剂残留
 2
 超高效液相色谱-串联质谱法测定蜂蜜中甲硝唑
 2
 超声辅助分散液相微萃取-高效液相色谱法测定蜂蜜中的咖啡因
 2
 粗SiC颗粒对再结晶碳化硅陶瓷抗热震性能的影响
 2
 多壁碳纳米管分散固相萃取-液相色谱-串联质谱法测定茶叶中5种烟碱类农药的残留量
 2
 分散固相萃取-气相色谱-质谱法测定地表水中的3种拟除虫菊酯含量
 2
 分散固相萃取-气相色谱-质谱法测定地表水中的异味物质
 2
 分散固相萃取-气相色谱-质谱法测定罐头食品中6种邻苯二甲酸酯
 2
 分散固相萃取-液相色谱-串联质谱法测定茶叶中12种农药的含量
 2
 傅里叶变换红外光谱法快速鉴别掺假蜂蜜
 2
 高效液相色谱法测定虾肉及虾制品中吲哚含量
 2
 高效液相色谱法测定氧化型染发剂中11种染料
 2
 气相色谱法测定茶叶中八氯二丙醚(S-421)残留量
 2
 气相色谱法测定茶叶中克螨特、哒螨酮残留量
 2
 同步荧光光谱法测定蜂蜜中游离氨基酸
 2
 液相色谱-串联质谱法测定洋葱中灭多威和杀线威残留量
 2