超高效液相色谱法测定水产品中喹乙醇的残留量
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摘要
称取经粉碎并匀浆后的水产样品(5.00±0.05)g,先后用水12mL及8mL在60℃水浴中提取2次,每次10min。离心分离,合并2次提取液。向提取液中加入饱和硼砂溶液9mL和300g·L-1硫酸锌溶液3mL,充分混匀进行脱色和除去杂质。离心分离,取上清液,通过固相萃取柱(SPE)使被测组分吸附在柱上,SPE柱用5mL水淋洗,弃去淋洗液。用甲醇-乙酸乙酯(10+90)混合液10mL将被测组分从柱上洗脱。收集洗脱液并在50℃条件下吹氮至近干,残渣用色谱分离所用的流动相1.0mL溶解,以下按色谱条件操作。用BEH C18色谱柱为固定相,甲醇-水(15+85)混合液为流动相进行色谱分离;用紫外检测器,检测波长为380nm。结果表明:喹乙醇的质量浓度在0.150～50.0mg·L-1内与其峰面积之间呈线性关系,检出限(3S/N)为30μg·kg-1。用标准加入法进行回收试验,测得回收率在76.4%～90.2%之间,测定值的相对标准偏差(n=5)在3.3%～9.0%之间。
Aquatic sample was minced,pulped and homogenized to a gruel-like state.A portion(5.00±0.05)g of the sample was taken and extracted twice with 12 mL and 8 mL of water at 60 ℃ for 10 min in each extraction.After centrifuging,the extracts were combined,decolorized and separated from some impurities by mixing with 9 mL of saturated borax solution and 3 mL of 300 g·L-1 zinc sulfate solution.The mixture was centrifugated,and the supernatant was taken and passed through SPE column to have the analyte(OLA)adsorbed on the column.The column was rinsed with 5 mL of water which were discarded.Then the column was eluted with10 mL of a mixture of methanol and ethyl acetate(10+90)to desorb OLA from the column.The eluate was collected and evaporated to near dryness by N2-blowing at 50 ℃.The residue was dissolved with 1.0 mL of the mobile phase used in UPLC analysis,and the solution was used for UPLC separation and determination.BEH C18 column was used as the stationary phase and a mixture of CH3 OH-H2 O(15+85)was used as mobile phase in the LC separation.UV detector was used in the detection at the wavelength of 380 nm.Linear relationship between values of peak area and mass concentration of OLA in the range of 0.150-50.0 mg·L-1 was obtained,with detection limit(3 S/N)of 30μg·kg-1.Recovery was tested by standard addition method,giving values of recovery ranged from 76.4%to 90.2%.Values of RSDs(n=5)were found in the range of 3.3%-9.0%.
Aquatic sample was minced,pulped and homogenized to a gruel-like state.A portion(5.00±0.05)g of the sample was taken and extracted twice with 12 mL and 8 mL of water at 60 ℃ for 10 min in each extraction.After centrifuging,the extracts were combined,decolorized and separated from some impurities by mixing with 9 mL of saturated borax solution and 3 mL of 300 g·L-1 zinc sulfate solution.The mixture was centrifugated,and the supernatant was taken and passed through SPE column to have the analyte(OLA)adsorbed on the column.The column was rinsed with 5 mL of water which were discarded.Then the column was eluted with10 mL of a mixture of methanol and ethyl acetate(10+90)to desorb OLA from the column.The eluate was collected and evaporated to near dryness by N2-blowing at 50 ℃.The residue was dissolved with 1.0 mL of the mobile phase used in UPLC analysis,and the solution was used for UPLC separation and determination.BEH C18 column was used as the stationary phase and a mixture of CH3 OH-H2 O(15+85)was used as mobile phase in the LC separation.UV detector was used in the detection at the wavelength of 380 nm.Linear relationship between values of peak area and mass concentration of OLA in the range of 0.150-50.0 mg·L-1 was obtained,with detection limit(3 S/N)of 30μg·kg-1.Recovery was tested by standard addition method,giving values of recovery ranged from 76.4%to 90.2%.Values of RSDs(n=5)were found in the range of 3.3%-9.0%.
引文
[1]田强兵,任惠丽,李锋刚,等.固相萃取-高效液相色谱法测定水产品中喹乙醇[J].分析试验室,2015,34(3):356-358.
[2]刘淳.超高效液相色谱测定猪肉中喹乙醇的残留量[J].分析仪器,2015(2):44-47.
[3]吕海鸾,吴聪明,程林丽,等.超高效液相色谱-串联质谱法检测畜产品和水产品中3-甲基喹噁啉-2-羧酸残留[J].色谱,2012,30(1):45-50.
[4]魏瑞成,包红朵,郑勤,等.粪源抗生素金霉素和喹乙醇在养殖水体中的残留及对锦鲤的生态毒理效应研究[J].农业环境科学学报,2009,28(9):1800-1805.
[5]杨先乐,胡鲲,邱军强,等.喹乙醇在鱼体内蓄积及其对鱼类的影响[J].水生生物学报,2005,29(1):13-19.
[6]陈海刚,李兆利,徐韵,等.三种兽药添加剂对赤子爱胜蚓体内纤维素酶和SOD酶的活性影响[J].南宁大学学报(自然科学版),2006,42(4):435-439.
[7] Commission Regulation(EC)No.2788/98.Official Journal of the European Communities,1998,L347(31/32):12-14.
[8]中国兽药典委员会.中国兽药典[M].北京:中国农业出版社,2005.
[9]李伟华.三聚氰胺、环丙沙星、喹乙醇和己烯雌酚残留的酶联免疫吸附检测法的建立[D].济南:山东大学,2010.
[10]谢小华,周德山,宋向明,等.高效液相色谱法测定水产品中喹乙醇残留量[J].理化检验-化学分册,2011,47(1):102-103.
[11] HU K,YANG X L.Determining olaquindox in fish tissue&feed by improved HPLC method(high performance liquid chromatography)[J].Journal of Shanghai Fisheries University,2003,12(S1):28-32.
[12]刘永涛,刘振红,丁运敏,等.HPLC-MS/MS同时测定水产品中喹烯酮、喹乙醇和5种大环内酯类抗生素残留[J].分析试验室,2010,29(8):44-47.
[13]钟仕花,郑雯,许远泉,等.超高效液相色谱-串联质谱法快速确证水产品中喹乙醇残留量[J].中国渔业质量与标准,2014,4(3):29-33.
[14] LYNCH M J,MOSHER F R,SCHNEIDER R P,et al.Determination of carbadox-related residues in swine liver by gas chromatography/mass spectrometry with ion trap detection[J].Journal Association of Official Analytical Chemists,1991,74(4):611-618.
[15] SC/T 3016-2004中华人民共和国水产行业标准水产品抽样方法[S].
[16]孔祥吉,王娜,徐静,等.斑马鱼体内喹乙醇的检测技术及富集特性研究[J].中国抗生素杂志,2016,41(1):55-59.
[17]梅景良,吴聪明,程林丽,等.HPLC法同步检测鲤鱼、对虾中喹乙醇与MQCA残留[J].海洋科学,2011,35(11):41-47.
[18]薛良辰,彭玉芬,刘陆,等.超高效液相色谱-串联质谱法快速检测水产品中喹乙醇及其代谢物3-甲基-喹噁啉-2-羟酸的残留[J].现代食品科技,2013,29(2):413-415.
[19]于慧娟,毕士川,黄冬梅,等.高效液相色谱法测定水产品中喹乙醇的残留量[J].分析科学学报,2004,20(3):281-283.
[20] SC/T 3019-2004中华人民共和国水产行业标准水产品中喹乙醇残留量的测定液相色谱法[S].
[2]刘淳.超高效液相色谱测定猪肉中喹乙醇的残留量[J].分析仪器,2015(2):44-47.
[3]吕海鸾,吴聪明,程林丽,等.超高效液相色谱-串联质谱法检测畜产品和水产品中3-甲基喹噁啉-2-羧酸残留[J].色谱,2012,30(1):45-50.
[4]魏瑞成,包红朵,郑勤,等.粪源抗生素金霉素和喹乙醇在养殖水体中的残留及对锦鲤的生态毒理效应研究[J].农业环境科学学报,2009,28(9):1800-1805.
[5]杨先乐,胡鲲,邱军强,等.喹乙醇在鱼体内蓄积及其对鱼类的影响[J].水生生物学报,2005,29(1):13-19.
[6]陈海刚,李兆利,徐韵,等.三种兽药添加剂对赤子爱胜蚓体内纤维素酶和SOD酶的活性影响[J].南宁大学学报(自然科学版),2006,42(4):435-439.
[7] Commission Regulation(EC)No.2788/98.Official Journal of the European Communities,1998,L347(31/32):12-14.
[8]中国兽药典委员会.中国兽药典[M].北京:中国农业出版社,2005.
[9]李伟华.三聚氰胺、环丙沙星、喹乙醇和己烯雌酚残留的酶联免疫吸附检测法的建立[D].济南:山东大学,2010.
[10]谢小华,周德山,宋向明,等.高效液相色谱法测定水产品中喹乙醇残留量[J].理化检验-化学分册,2011,47(1):102-103.
[11] HU K,YANG X L.Determining olaquindox in fish tissue&feed by improved HPLC method(high performance liquid chromatography)[J].Journal of Shanghai Fisheries University,2003,12(S1):28-32.
[12]刘永涛,刘振红,丁运敏,等.HPLC-MS/MS同时测定水产品中喹烯酮、喹乙醇和5种大环内酯类抗生素残留[J].分析试验室,2010,29(8):44-47.
[13]钟仕花,郑雯,许远泉,等.超高效液相色谱-串联质谱法快速确证水产品中喹乙醇残留量[J].中国渔业质量与标准,2014,4(3):29-33.
[14] LYNCH M J,MOSHER F R,SCHNEIDER R P,et al.Determination of carbadox-related residues in swine liver by gas chromatography/mass spectrometry with ion trap detection[J].Journal Association of Official Analytical Chemists,1991,74(4):611-618.
[15] SC/T 3016-2004中华人民共和国水产行业标准水产品抽样方法[S].
[16]孔祥吉,王娜,徐静,等.斑马鱼体内喹乙醇的检测技术及富集特性研究[J].中国抗生素杂志,2016,41(1):55-59.
[17]梅景良,吴聪明,程林丽,等.HPLC法同步检测鲤鱼、对虾中喹乙醇与MQCA残留[J].海洋科学,2011,35(11):41-47.
[18]薛良辰,彭玉芬,刘陆,等.超高效液相色谱-串联质谱法快速检测水产品中喹乙醇及其代谢物3-甲基-喹噁啉-2-羟酸的残留[J].现代食品科技,2013,29(2):413-415.
[19]于慧娟,毕士川,黄冬梅,等.高效液相色谱法测定水产品中喹乙醇的残留量[J].分析科学学报,2004,20(3):281-283.
[20] SC/T 3019-2004中华人民共和国水产行业标准水产品中喹乙醇残留量的测定液相色谱法[S].