超高效液相色谱联用三重四极杆质谱法同时测定蜂蜜中氯霉素、甲硝唑和林可霉素
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摘要
目的建立快速同时测定蜂蜜中氯霉素、甲硝唑和林可霉素残留量的超高效液相色谱联用三重四极杆质谱法。方法蜂蜜样品在pH=10下经乙酸乙酯萃取净化,以甲醇和0.1%氨水作为流动相进行梯度洗脱,在Acquity BEH C18(2.1 mm×50 mm,1.7μm)色谱柱上实现分离,采用电喷雾正负离子多反应监测模式扫描采集,稳定同位素稀释法测定氯霉素、甲硝唑和林可霉素的残留量。结果氯霉素在0.10～10.00μg/L、甲硝唑和林可霉素在0.05～10μg/L浓度范围内,呈线性关系,相关系数>0.999 0;氯霉素的检出限(LOD)和定量限(LOQ)分别为0.03μg/kg和0.10μg/kg,甲硝唑和林可霉素的LOD均为0.02μg/kg,LOQ均为0.05μg/kg;在蜂蜜中分别添加0.10μg/kg、0.30μg/kg和9.00μg/kg的氯霉素,各0.05μg/kg、0.3μg/kg和9.00μg/kg的甲硝唑和林可霉素,加标回收率为98.1%～110.0%,相对标准偏差(RSD)为1.4%～17.0%(n=6);6份市售蜂蜜样品中有1份检出林可霉素,含量为0.57μg/kg,其余样品均未检出。结论所建实验方法适合于蜂蜜中氯霉素、甲硝唑和林可霉素残留量的同时测定,具有灵敏、准确、简便的特点,可用于食品安全风险监测实际样品的测定。
引文
[1]曹艳平,辛成龙,季萍.同位素稀释气相色谱-三重四极杆质谱测定虾仁中氯霉素[J].分析科学学报,2015,31(4):545-547.
[2]高何刚,杜赛,王瑞,等.超高效液相色谱-串联质谱法测定蜂蜜中氯霉素和甲硝唑残留[J].预防医学,2017,29(9):969-972.
[3]HUANG X,LIN J,YUAN D.Simple and sensitive determination of nitroimidazole residues in honey using stir bar sorptive extraction with mixed mode monolith followed by liquid chromatography[J].Journal of Separation Science,2015,34(16-17):2138-2144.
[4]张璐,孔祥虹,何强,等.超高效液相色谱-串联质谱联用法对奶粉中3种硝基眯唑残留物的测定[J].分析测试学报,2010,29(3):306-309.
[5]WANG J.Determination of five macrolide antibiotic residues in honey by LC-ESI-MS and LC-ESI-MS/MS[J].Journal of Agricultural&Food Chemistry,2004,52(2):171-181.
[6]杜飞,杨永红,唐荣平,等.欧洲幼虫臭腐病概况[J].中兽医医药杂志,2007,26(1):66-67.
[7]PETTIS J S,FELDLAUFER M F.Efficacy of lincomycin and tylosin in controlling American foulbrood in honey bee colonies[J].Journal of Apicultural Research,2005,44(3):106-108.
[8]中华人民共和国农业部.食品动物禁用的兽药及其它化合物清单[EB/OL].(2011-04-22)[2018-09-29].http://jiuban.moa.gov.cn/zwllm/tzgg/gg/201104/t20110422_1976324.htm.
[9]刘伟,张楠,李兵,等.固相萃取-超高效液相色谱-同位素稀释串联质谱法测定蜂蜜中的甲硝唑和氯霉素[J].分析科学学报,2017,33(1):145-148.
[10]图雅,崔建平,赵宏.同位素内标-超高效液相色谱-串联质谱法测定蜂蜜中氯霉素及甲硝唑[J].中国食品卫生杂志,2017,29(4):450-453.
[11]肖国军,蔡超海,王生,等.固相萃取高效液相色谱串联质谱法同时测定蜂蜜中甲硝唑、氯霉素、甲砜霉素和氟甲砜霉素残留[J].中国卫生检验杂志,2018,28(1):22-25.
[12]章剑,李昌安,李建伟,等.固相萃取-超高效液相色谱-串联质谱法同时测定蜂蜜样品中氯霉素和甲硝唑[J].安徽预防医学杂志,2018,24(1):16-20.
[13]徐锦忠,吴斌,丁涛,等.高效液相色谱-电喷雾串联质谱法测定蜂蜜中的林可胺类抗生素残留[J].色谱,2006,24(5):436-439.
[14]林洁,曹建明,蔡欣欣,等.超高效液相色谱三重四极杆质谱法快速测定蜂蜜中12种大环内酯和林可酰胺类药物残留[J].中国卫生检验杂志,2010,20(5):959-962.
[15]MATUSZEWSKI B K,CONSTANZER M L,CHAVEZ-ENG C M.Strategies for the assessment of matrix effect in quantitative bioanalytical methods based on HPLC-MS/MS[J].Anal Chem,2003,75(13):3019-3030.
[2]高何刚,杜赛,王瑞,等.超高效液相色谱-串联质谱法测定蜂蜜中氯霉素和甲硝唑残留[J].预防医学,2017,29(9):969-972.
[3]HUANG X,LIN J,YUAN D.Simple and sensitive determination of nitroimidazole residues in honey using stir bar sorptive extraction with mixed mode monolith followed by liquid chromatography[J].Journal of Separation Science,2015,34(16-17):2138-2144.
[4]张璐,孔祥虹,何强,等.超高效液相色谱-串联质谱联用法对奶粉中3种硝基眯唑残留物的测定[J].分析测试学报,2010,29(3):306-309.
[5]WANG J.Determination of five macrolide antibiotic residues in honey by LC-ESI-MS and LC-ESI-MS/MS[J].Journal of Agricultural&Food Chemistry,2004,52(2):171-181.
[6]杜飞,杨永红,唐荣平,等.欧洲幼虫臭腐病概况[J].中兽医医药杂志,2007,26(1):66-67.
[7]PETTIS J S,FELDLAUFER M F.Efficacy of lincomycin and tylosin in controlling American foulbrood in honey bee colonies[J].Journal of Apicultural Research,2005,44(3):106-108.
[8]中华人民共和国农业部.食品动物禁用的兽药及其它化合物清单[EB/OL].(2011-04-22)[2018-09-29].http://jiuban.moa.gov.cn/zwllm/tzgg/gg/201104/t20110422_1976324.htm.
[9]刘伟,张楠,李兵,等.固相萃取-超高效液相色谱-同位素稀释串联质谱法测定蜂蜜中的甲硝唑和氯霉素[J].分析科学学报,2017,33(1):145-148.
[10]图雅,崔建平,赵宏.同位素内标-超高效液相色谱-串联质谱法测定蜂蜜中氯霉素及甲硝唑[J].中国食品卫生杂志,2017,29(4):450-453.
[11]肖国军,蔡超海,王生,等.固相萃取高效液相色谱串联质谱法同时测定蜂蜜中甲硝唑、氯霉素、甲砜霉素和氟甲砜霉素残留[J].中国卫生检验杂志,2018,28(1):22-25.
[12]章剑,李昌安,李建伟,等.固相萃取-超高效液相色谱-串联质谱法同时测定蜂蜜样品中氯霉素和甲硝唑[J].安徽预防医学杂志,2018,24(1):16-20.
[13]徐锦忠,吴斌,丁涛,等.高效液相色谱-电喷雾串联质谱法测定蜂蜜中的林可胺类抗生素残留[J].色谱,2006,24(5):436-439.
[14]林洁,曹建明,蔡欣欣,等.超高效液相色谱三重四极杆质谱法快速测定蜂蜜中12种大环内酯和林可酰胺类药物残留[J].中国卫生检验杂志,2010,20(5):959-962.
[15]MATUSZEWSKI B K,CONSTANZER M L,CHAVEZ-ENG C M.Strategies for the assessment of matrix effect in quantitative bioanalytical methods based on HPLC-MS/MS[J].Anal Chem,2003,75(13):3019-3030.