液相质谱法同时检测猪肉中氯霉素和地塞米松
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摘要
建立一种利用高效液相色谱-串联质谱法同时检测猪肉中氯霉素和地塞米松药物残留的方法。猪肉样品中的药物残留经乙酸乙酯提取后,经氮气吹干,残渣溶解后过Silica柱,洗脱液经氮气吹干,用初始流动相溶解定容。用Shim-pack GIST C18色谱柱(150 mm×2.1 mm,5μm)分离,以纯水-甲醇为流动相进行梯度洗脱,质谱采用多反应监测模式,氯霉素以内标法定量,地塞米松以外标法定量。在5 min内完成了两种目标化合物的分离分析。氯霉素和地塞米松在0.2μg/kg～40μg/kg范围内线性关系良好,相关系数r2分别为0.999 9和0.999 7。氯霉素添加水平在1、2.5、5μg/kg时,回收率在90.54%～101.73%之间;地塞米松添加量在0.5、2.5、5μg/kg时,回收率在83.82%～87.5%之间;批内标准偏差和批间标准偏差均小于10%(n=5),方法定量限均小于0.15μg/kg。
A method for simultaneous determination of chloramphenicol and dexamethasone residues in pork tissues by liquid chromatography-tandem mass spectrometry(LC-MS/MS)was established. The residues in pork samples were extracted by ethyl acetate and dried by nitrogen. The residues were dissolved and passed over the Silica columns,the eluents were dried by nitrogen and metered volume by initial flow. The liquid was performed on a Shim-pack GIST C18 chromatographic column with gradient elution of pure water and methanol. The mass spectrometry was carried out with multiple reaction monitoring,chloramphenicol was quantified by internal standard method and dexamethasone was quantified by external standard method. The separation and analysis of two target compounds was completed within 5 min. Chloramphenicol and dexamethasone showed good linear relationships in the concentration range of 0.2 μg/kg to 40 μg/kg with the correlation coefficients of 0.999 9 and 0.999 7 respectively. The recovery of chloramphenicol at 3 spiked levels(1,2.5,5μg/kg)was 90.54 %-101.73 % and the recovery of dexamethasone at 3 spiked levels(0.5,2.5,5 μg/kg)was 83.82 %-87.5 %.The standard deviations of the same batch and 3 batches were less than 10 %(n=5),the quantitation limits of two target compounds were less than 0.15 μg/kg.
A method for simultaneous determination of chloramphenicol and dexamethasone residues in pork tissues by liquid chromatography-tandem mass spectrometry(LC-MS/MS)was established. The residues in pork samples were extracted by ethyl acetate and dried by nitrogen. The residues were dissolved and passed over the Silica columns,the eluents were dried by nitrogen and metered volume by initial flow. The liquid was performed on a Shim-pack GIST C18 chromatographic column with gradient elution of pure water and methanol. The mass spectrometry was carried out with multiple reaction monitoring,chloramphenicol was quantified by internal standard method and dexamethasone was quantified by external standard method. The separation and analysis of two target compounds was completed within 5 min. Chloramphenicol and dexamethasone showed good linear relationships in the concentration range of 0.2 μg/kg to 40 μg/kg with the correlation coefficients of 0.999 9 and 0.999 7 respectively. The recovery of chloramphenicol at 3 spiked levels(1,2.5,5μg/kg)was 90.54 %-101.73 % and the recovery of dexamethasone at 3 spiked levels(0.5,2.5,5 μg/kg)was 83.82 %-87.5 %.The standard deviations of the same batch and 3 batches were less than 10 %(n=5),the quantitation limits of two target compounds were less than 0.15 μg/kg.
引文
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[2]张亚莉,哈婧,赵静,等.动物组织中抗生素残留研究进展[J].河北科技大学学报,2013,34(6):517-525
[3]曹巧玲,杨凯,武泽新.氯霉素的毒性作用和检测方法研究进展[J].职业与健康,2013,29(16):2095-2097
[4]王秀,杨新立,孟勇.氯霉素在畜禽体内残留问题的研究进展[J].当代畜禽养殖业,2011(2):3-6
[5]Guillaume Binson,NicolasVenisse,Astrid Bacle,et al.Preparation and Physico-Chemical Stability of Dexamethasone Oral Suspension[J].Pharmaceutical Technology in Hospital Pharmacy,2018,2(4):193-201
[6]刘文卫,钮伟民,许伟芳.氯霉素残留检测技术的研究进展[J].现代预防医学,2007(1):67-68,75
[7]国家药典委员会.中华人民共和国药典:2010年版:第一增补本[M].北京:中国医药科技出版社,2010
[8]刘岩,王艳鸽,张鑫.食品中抗生素检测技术研究进展[J].山西食品工业,2005(3):38-41,43
[9]张丽芳,薛飞群.液质联用法测定血浆中罗红霉素的内标法与外标法的比较[J].分析试验室,2009,28(S2):66-69
[10]张震,张俊,闫跃飞,等.液相色谱串联质谱内标法与外标法检测生鲜乳中黄曲霉素M1含量的比较[J].黑龙江畜牧兽医,2018(13):211-214