高效液相色谱/串联质谱法研究溴氰菊酯在中华绒螯蟹体内的富集消除规律
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摘要
本研究建立了中华绒螯蟹(Eriocheir sinensis)体内溴氰菊酯残留的液相色谱/串联质谱检测方法,并选择溴氰菊酯对中华绒螯蟹的安全质量浓度0.66μg/L,在(20±1)℃下,对中华绒螯蟹进行浸浴,研究溴氰菊酯在中华绒螯蟹体内的富集消除规律。样品经乙腈提取,采用电喷雾正离子源(ESI~+)和多重反应监测(MRM)模式测定,基质匹配标准曲线定量。结果表明,溴氰菊酯标准曲线在0.1～50.0μg/L质量浓度线性关系良好,决定系数为0.999 8,检测限为0.035μg/L。0.10μg/kg(μg/L)、10.00μg/kg(μg/L)、20.00μg/kg(μg/L)和50.00μg/kg(μg/L)添加水平下,溴氰菊酯回收率为82.63%～101.00%。各组织对溴氰菊酯的富集能力不同,其中血淋巴和鳃富集能力较强。血淋巴、肝胰腺和鳃等组织中药物质量浓度同时达到峰值,达到峰值时间(T_(max))为0.5 h,峰值质量浓度或质量分数(C_(max))分别为2.780μg/L,0.567μg/kg和1.165μg/kg。为了最大限度地避免溴氰菊酯残留对人体造成的危害,除了选择中华绒螯蟹重要的可食组织肝胰腺作为检测对象外,还应选择血淋巴等组织进行进一步的药残检测。
A method for the determination of deltamethrin in Eriocheir sinensis by liquid chromatography/tandem mass spectrometry was established. The crabs were given a immersion bath in the safe concentration of deltamethrin at the dose of 0.66 μg/L and temperature of(20±1) ℃ to investigate the rule of accumulation and elimination of deltamethrin in E. sinensis. The samples were extracted by acetonitrile. Electrospray positive ion source(ESI~+), multiple reaction monitoring mode(MRM) and matrix-matched external standard method were applied to sample analysis. Results indicated that the standard curve of deltamethrin was in good linearity in the range of 0.1-50.0 μg/L, the coefficient of determination was 0.999 8, and the detection limit was 0.035 μg/L. The recoveries for deltamethrin at the addition of 0.10 μg/kg(μg/L), 10.00 μg/kg(μg/L), 20.00 μg/kg(μg/L) and 50.00 μg/kg(μg/L) ranged from 82.63% to 101.00%. The enrichment capacities of different tissues of E. sinensis for deltamethrin were different, the capacities of hemolymph and gills were comparatively stronger. The concentrations of deltamethrin in hemolymph, hepatopancreas and gills reached their C_(max)(2.780 μg/L, 0.567 μg/kg and 1.165 μg/kg) at the same time at 0.5 h(T_(max)). In order to avoid the harm caused by deltamethrin residue to the human body, the hemolymph and other tissues should be also selected as the object of drug residue detection except for hepatopancreas, which is the important edible tissue of E. sinensis.
A method for the determination of deltamethrin in Eriocheir sinensis by liquid chromatography/tandem mass spectrometry was established. The crabs were given a immersion bath in the safe concentration of deltamethrin at the dose of 0.66 μg/L and temperature of(20±1) ℃ to investigate the rule of accumulation and elimination of deltamethrin in E. sinensis. The samples were extracted by acetonitrile. Electrospray positive ion source(ESI~+), multiple reaction monitoring mode(MRM) and matrix-matched external standard method were applied to sample analysis. Results indicated that the standard curve of deltamethrin was in good linearity in the range of 0.1-50.0 μg/L, the coefficient of determination was 0.999 8, and the detection limit was 0.035 μg/L. The recoveries for deltamethrin at the addition of 0.10 μg/kg(μg/L), 10.00 μg/kg(μg/L), 20.00 μg/kg(μg/L) and 50.00 μg/kg(μg/L) ranged from 82.63% to 101.00%. The enrichment capacities of different tissues of E. sinensis for deltamethrin were different, the capacities of hemolymph and gills were comparatively stronger. The concentrations of deltamethrin in hemolymph, hepatopancreas and gills reached their C_(max)(2.780 μg/L, 0.567 μg/kg and 1.165 μg/kg) at the same time at 0.5 h(T_(max)). In order to avoid the harm caused by deltamethrin residue to the human body, the hemolymph and other tissues should be also selected as the object of drug residue detection except for hepatopancreas, which is the important edible tissue of E. sinensis.
引文
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[10] SHEN H S,ZANG Y N,SONG K,et al.A meta-transcriptomics survey reveals changes in the microbiota of the Chinese mitten crab Eriocheir sinensis infected with hepatopancreatic necrosis disease[J].Frontiers in Microbiology,2017,8:732.
[11] SHARMA P,ASLAM K I,SINGH R.Curcumin and quercetin ameliorated cypermethrin and deltamethrin-induced reproductive system impairment in male wistar rats by upregulating the activity of pituitary-gonadal hormones and steroidogenic enzymes[J].International Journal of Fertility & Sterility,2018,12(1):72-80.
[12] SAOUDI M,BADRAOUI R,BOUHAJJA H,et al.Deltamethrin induced oxidative stress in kidney and brain of rats:protective effect of Artemisia campestris essential oil[J].Biomedicine & Pharmacotherapy,2017,94:955-963.
[13] 中华人民共和国农业部.绿色食品蟹:NY/T 841—2012[S].北京:中国农业出版社,2012.
[14] 林丽聪.溴氰菊酯在欧洲鳗鲡体内药代动力学研究[J].福建水产,2008(2):33-36.
[15] 徐春娟,刘永涛,艾晓辉,等.溴氰菊酯在团头鲂体内的富集消除规律研究[J].西北农林科技大学学报,2017,45(12):1-7.
[16] 杨宗英,张一柳,胡鲲,等.溴氰菊酯对中华绒螯蟹肝胰腺氧化胁迫效应和组织结构的影响[J].浙江农业学报,2017,29(8):1261-1270.
[17] 汪建国,王玉堂,陈昌福.渔药药效学[M].北京:中国农业出版社,2011:84-85.
[18] 郭涛.临床药代动力学理论与实践——创伤治疗药物[M].北京:人民军医出版社,2014:36-39.
[19] 王为中,崔世海,闫婷婷,等.磁固相萃取与高效液相色谱联用测定水体中防治白蚁农药残留[J].南京师大学报(自然科学版),2016,39(4):132-138.
[20] 杨韶松,陈静,唐旭斌.香料烟中2种菊酯农药的残留降解动态[J].华中农业大学学报,2013,32(1):68-72.
[21] 吴南村,张群,刘春华,等.凝胶渗透色谱/固相萃取净化-气相色谱-串联质谱检测白胡椒中的毒死蜱和溴氰菊酯残留[J].农药,2016,55(12):903-905.
[22] 王恒玲,李敏,李培武,等.油菜薹中醚菊酯酶联免疫(ELISA)快速检测方法建立[J].中国油料作物学报,2015,37(3):354-359.
[23] KAUFMAN B M,JR C M.Immunoassay of pesticides[J].Journal-Association of Official Analytical Chemists,1991,74(2):239.
[24] 耿雪冰.溴氰菊酯残留的检测方法及对河蟹的毒性研究[D].南京:南京农业大学,2010:21-27.
[25] ZHENG Z L,ZHANG S Y,MA W D,et al.Determination of dexmedetomidine by UHPLC-MS/MS and its application to evaluate the effect of dexmedetomidine concentration on the target-controlled infusion concentration of propofol[J].Journal of Pharmaceutical and Biomedical Analysis,2018,154:438-443.
[26] 中华人民共和国农业部.农业部[2003]1号文件,关于颁布《农业部兽药残留试验技术规范(试行)》的通知[Z].2003.
[27] HALLY B A,NESSEL R J,LU A Y H.Ivermectin and abamectin[M].New York:Springer,1989:162-200.
[28] ARSLAN H,ALTUN S,?ZDEMIR S.Acute toxication of deltamethrin results in activation of iNOS,8-OHdG and up-regulation of caspase 3,iNOS gene expression in common carp (Cyprinus carpio L.)[J].Aquatic Toxicology,2017,187:90.
[29] YANG Z,ZHANG Y,JIANG Y,et al.Transcriptional responses in the hepatopancreas of Eriocheir sinensis exposed to deltamethrin[J].PLoS ONE,2017,12(9):e0184581.
[30] 邢丽红,孙伟红,冷凯良,等.阿维菌素在鲈组织中的富集及消除规律研究[J].中国渔业质量与标准,2013,3(4):63-69.
[31] 梁楠,胡鲲,刘腾飞,等.亚甲基蓝及其代谢物在异育银鲫体内分布及消除规律的研究[J].南方水产科学,2017,13(1):19-25.
[32] 鞠晶,王伟利,姜兰,等.磺胺间甲氧嘧啶在罗非鱼体内的药物代谢动力学及休药期[J].华中农业大学学报,2015,34(1):103-107.
[33] DAVIES N M,TAKEMOTO J K,BROCKS D R,et al.Multiple peaking phenomena in pharmacokinetic disposition [J].Clinical Pharmacokinetics,2010,49(6):351-377.
[34] STAPPAERTS J,ANNAERT P,AUGUSTIJNS P.Site dependent intestinal absorption of darunavir and its interaction with ketoconazole [J].European Journal of Pharmaceutical Sciences,2013,49(1):51.
[35] WADA S,KANO T,MITA S,et al.The role of inter-segmental differences in p-glycoprotein expression and activity along the rat small intestine in causing the double-peak phenomenon of substrate plasma concentration [J].Drug Metabolism & Pharmacokinetics,2013,28(2):98-103.
[36] ROBERTS M S,MAGNUSSON B M,BURCZYNSKI F J,et al.Enterohepatic circulation:physiological,pharmacokinetic and clinical implications [J].Clinical Pharmacokinetics,2002,41(10):751.
[2] SINGH S,TIWARI R K,PANDEY R S.Evaluation of acute toxicity of triazophos and deltamethrin and their inhibitory effect on AChE activity in Channa punctatus [J].Toxicology Reports,2018,5:85-89.
[3] 张新铖,朱新平,刘毅辉,等.甲苯咪唑、溴氰菊酯和硫酸铜对美洲鲥的急性毒性研究[J].南方水产科学,2015,11(2):66-71.
[4] ELLIOTT M,FARNHAM A W,JANES N F,et al.Synthetic insecticide with a new order of activity[J].Nature,1974,248(450):710-711.
[5] 胡笑形.我国农药工业的现状与发展方向[J].农药,1998,37(6):7-10.
[6] LIU X,ZHANG Q,LI S,et al.Developmental toxicity and neurotoxicity of synthetic organic insecticides in zebrafish (Danio rerio):a comparative study of deltamethrin,acephate,and thiamethoxam[J].Chemosphere,2018,199:16-25.
[7] TOUMI H,BOUMAIZA M,MILLET M,et al.Effects of deltamethrin (pyrethroid insecticide) on growth,reproduction,embryonic development and sex differentiation in two strains of Daphnia magna (Crustacea,Cladocera)[J].Science of the Total Environment,2013,458-460:47-53.
[8] JACQUELINE C M,CRISTIAN G E.Deltamethrin (AlphaMaxTM) reveals modulation of genes related to oxidative stress in the ectoparasite Caligus rogercresseyi:Implications on delousing drug effectiveness[J].Aquaculture,2014,433(37):421-429.
[9] DING Z,MENG Q,LIU H,et al.First case of hepatopancreatic necrosis disease in pond-reared Chinese mitten crab,Eriocheir sinensis,associated with microsporidian[J].Journal of Fish Disease,2016,39(9):1043-1051.
[10] SHEN H S,ZANG Y N,SONG K,et al.A meta-transcriptomics survey reveals changes in the microbiota of the Chinese mitten crab Eriocheir sinensis infected with hepatopancreatic necrosis disease[J].Frontiers in Microbiology,2017,8:732.
[11] SHARMA P,ASLAM K I,SINGH R.Curcumin and quercetin ameliorated cypermethrin and deltamethrin-induced reproductive system impairment in male wistar rats by upregulating the activity of pituitary-gonadal hormones and steroidogenic enzymes[J].International Journal of Fertility & Sterility,2018,12(1):72-80.
[12] SAOUDI M,BADRAOUI R,BOUHAJJA H,et al.Deltamethrin induced oxidative stress in kidney and brain of rats:protective effect of Artemisia campestris essential oil[J].Biomedicine & Pharmacotherapy,2017,94:955-963.
[13] 中华人民共和国农业部.绿色食品蟹:NY/T 841—2012[S].北京:中国农业出版社,2012.
[14] 林丽聪.溴氰菊酯在欧洲鳗鲡体内药代动力学研究[J].福建水产,2008(2):33-36.
[15] 徐春娟,刘永涛,艾晓辉,等.溴氰菊酯在团头鲂体内的富集消除规律研究[J].西北农林科技大学学报,2017,45(12):1-7.
[16] 杨宗英,张一柳,胡鲲,等.溴氰菊酯对中华绒螯蟹肝胰腺氧化胁迫效应和组织结构的影响[J].浙江农业学报,2017,29(8):1261-1270.
[17] 汪建国,王玉堂,陈昌福.渔药药效学[M].北京:中国农业出版社,2011:84-85.
[18] 郭涛.临床药代动力学理论与实践——创伤治疗药物[M].北京:人民军医出版社,2014:36-39.
[19] 王为中,崔世海,闫婷婷,等.磁固相萃取与高效液相色谱联用测定水体中防治白蚁农药残留[J].南京师大学报(自然科学版),2016,39(4):132-138.
[20] 杨韶松,陈静,唐旭斌.香料烟中2种菊酯农药的残留降解动态[J].华中农业大学学报,2013,32(1):68-72.
[21] 吴南村,张群,刘春华,等.凝胶渗透色谱/固相萃取净化-气相色谱-串联质谱检测白胡椒中的毒死蜱和溴氰菊酯残留[J].农药,2016,55(12):903-905.
[22] 王恒玲,李敏,李培武,等.油菜薹中醚菊酯酶联免疫(ELISA)快速检测方法建立[J].中国油料作物学报,2015,37(3):354-359.
[23] KAUFMAN B M,JR C M.Immunoassay of pesticides[J].Journal-Association of Official Analytical Chemists,1991,74(2):239.
[24] 耿雪冰.溴氰菊酯残留的检测方法及对河蟹的毒性研究[D].南京:南京农业大学,2010:21-27.
[25] ZHENG Z L,ZHANG S Y,MA W D,et al.Determination of dexmedetomidine by UHPLC-MS/MS and its application to evaluate the effect of dexmedetomidine concentration on the target-controlled infusion concentration of propofol[J].Journal of Pharmaceutical and Biomedical Analysis,2018,154:438-443.
[26] 中华人民共和国农业部.农业部[2003]1号文件,关于颁布《农业部兽药残留试验技术规范(试行)》的通知[Z].2003.
[27] HALLY B A,NESSEL R J,LU A Y H.Ivermectin and abamectin[M].New York:Springer,1989:162-200.
[28] ARSLAN H,ALTUN S,?ZDEMIR S.Acute toxication of deltamethrin results in activation of iNOS,8-OHdG and up-regulation of caspase 3,iNOS gene expression in common carp (Cyprinus carpio L.)[J].Aquatic Toxicology,2017,187:90.
[29] YANG Z,ZHANG Y,JIANG Y,et al.Transcriptional responses in the hepatopancreas of Eriocheir sinensis exposed to deltamethrin[J].PLoS ONE,2017,12(9):e0184581.
[30] 邢丽红,孙伟红,冷凯良,等.阿维菌素在鲈组织中的富集及消除规律研究[J].中国渔业质量与标准,2013,3(4):63-69.
[31] 梁楠,胡鲲,刘腾飞,等.亚甲基蓝及其代谢物在异育银鲫体内分布及消除规律的研究[J].南方水产科学,2017,13(1):19-25.
[32] 鞠晶,王伟利,姜兰,等.磺胺间甲氧嘧啶在罗非鱼体内的药物代谢动力学及休药期[J].华中农业大学学报,2015,34(1):103-107.
[33] DAVIES N M,TAKEMOTO J K,BROCKS D R,et al.Multiple peaking phenomena in pharmacokinetic disposition [J].Clinical Pharmacokinetics,2010,49(6):351-377.
[34] STAPPAERTS J,ANNAERT P,AUGUSTIJNS P.Site dependent intestinal absorption of darunavir and its interaction with ketoconazole [J].European Journal of Pharmaceutical Sciences,2013,49(1):51.
[35] WADA S,KANO T,MITA S,et al.The role of inter-segmental differences in p-glycoprotein expression and activity along the rat small intestine in causing the double-peak phenomenon of substrate plasma concentration [J].Drug Metabolism & Pharmacokinetics,2013,28(2):98-103.
[36] ROBERTS M S,MAGNUSSON B M,BURCZYNSKI F J,et al.Enterohepatic circulation:physiological,pharmacokinetic and clinical implications [J].Clinical Pharmacokinetics,2002,41(10):751.
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