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当前位置: 首页 > 文章 > 高效液相色谱-串联质谱法检测鹌鹑蛋及鸽蛋中氯霉素类药物残留 扬州大学学报(农业与生命科学版) 2019 (6) 86-92
Position: Home > Articles > Study on determination of chloramphenicol residues in quail eggs and pigeon eggs by high performance liquid chromatography-tandem mass spectrometry Journal of Yangzhou University(Agricultural and Life Science Edition) 2019 (6) 86-92

高效液相色谱-串联质谱法检测鹌鹑蛋及鸽蛋中氯霉素类药物残留

作  者：
奚照寿;陈长宽;袁华根;沈建新;丁丽军
单  位：
江苏沿海地区农业科学研究所;江苏农牧科技职业学院;常熟市支塘动物防疫站
关键词：
鹌鹑蛋;鸽蛋;氯霉素类药物;残留;高效液相色谱-串联质谱法
摘  要：
为建立鹌鹑蛋和鸽蛋中氯霉素(CAP)、甲砜霉素(TAP)、氟苯尼考(FF)及其代谢产物氟苯尼考胺(FFA)多残留同时检测的高效液相色谱-串联质谱法,以乙酸乙酯、乙腈、氨水溶液(体积比为49∶49∶2)提取、净化样品,乙腈饱和的正己烷去脂,用高效液相色谱-串联质谱(HPLC-MS/MS)仪进行分析。以多反应监测模式(MRM)运行,采用正、负离子模式下电喷雾电离,内标法定量,以2 mmol·L~(-1)乙酸铵-水和2 mmol·L~(-1)乙酸铵-乙腈溶液为流动相。结果表明:CAP、TAP、FF和FFA分别在0.1～25.0、1.0～150.0、0.3～250.0、1.5～250.0μg·kg~(-1)浓度范围内,线性关系良好,决定系数均在0.999 3以上。4种药物添加水平为定量限、0.5 MRL、1 MRL和2 MRL时,平均回收率为89.30%～105.41%,相对标准偏差均低于3.87%。4种药物的检测限和定量限范围分别为0.04～0.50和0.1～1.5μg·kg~(-1)。
译  名：
Study on determination of chloramphenicol residues in quail eggs and pigeon eggs by high performance liquid chromatography-tandem mass spectrometry
作  者：
XI Zhaoshou;CHEN Changkuan;YUAN Huagen;SHEN Jianxin;DING Lijun;Jiangsu Agri-Animal Husbandry Vocational College;Institute of Agricultural Sciences in Jiangsu Coastal Areas;Changshu Zhitang Animal Epidemic Prevention Station;
关键词：
quail eggs;;pigeon eggs;;chloramphenicols;;residue;;high performance liquid chromatography-tandem mass spectrometry
摘  要：
A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) method was developed for the simultaneous detection of chloramphenicol(CAP), thiamphenicol(TAP), florfenicol(FF) and its metabolite florfenicol amine(FFA) in quail eggs and pigeon eggs. The sample was extracted with ethyl acetate∶acetonitrile∶aqueous ammonia solution(49∶49∶2, V/V), and degreased with acetonitrile-saturated n-hexane and subjected to HPLC-MS/MS analysis. The system was run in multiple reaction monitoring(MRM) mode, using electrospray ionization in positive and negative ion mode and quantified by internal standard method. The mobile phase was composed of water and acetonitrile, both containing 2 mmol·L~(-1) of ammonium acetate. The results showed that CAP, TAP, FF and FFA were in the range of 0.1-25.0, 1.0-150.0, 0.3-250.0 and 1.5-250.0 μg·kg~(-1), respectively, the linear relationship was good, and the determination coefficient was above 0.999 3. When the added concentration of the four drugs were limits of quantitation(LOQs), 0.5 MRL, 1 MRL and 2 MRL, the average recovery was 89.30%-105.41%, and the relative standard deviation was lower than 3.87%. The limits of detection(LODs) and LOQs for the four drugs ranged from 0.04 to 0.50 and 0.1 to 1.5 μg·kg~(-1), respectively.

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