高效液相色谱-串联质谱法测定蜂蜡中痕量氯霉素残留  

Determination of trace chloramphenicol residue in beeswax by high performance liquid chromatography tandem mass spectrometry

作　　者：雷美康 候建波 祝子铜 王笑笑 章应俊 许赢升 彭芳 LEI Mei-Kang;HOU Jian-Bo;ZHU Zi-Tong;WANG Xiao-Xiao;ZHANG Ying-Jun;XU Ying-Shen;PENG Fang(Technical Center of Hangzhou Customs,Hangzhou 310016,China;The Comprehensive Technology and Service Center of Quzhou Customs,Quzhou 324003,China;Quzhou Institute for Food and Drug Control,Quzhou 324003,China)

机构地区：[1]杭州海关技术中心,杭州310016 [2]衢州海关综合技术服务中心,衢州324003 [3]衢州市食品药品检验研究院,衢州324003

出　　处：《食品安全质量检测学报》2021年第3期1088-1092,共5页Journal of Food Safety and Quality

基　　金：衢州市科技计划项目(2020K47)。

摘　　要：目的建立正己烷预处理-固相萃取净化-高效液相色谱-串联质谱法检测蜂蜡中痕量氯霉素的分析方法。方法试样采用正己烷预溶解,经水提取后进行亲水亲脂平衡(hydrophilic-lipophilic-balance, HLB)固相萃取小柱净化,用Accucore XL C18柱分离,多反应监测(multiple reaction monitoring, MRM)模式串联质谱进行测定,内标法定量。结果氯霉素在0.3~10 ng/mL范围内与峰面积具有较好的线性关系,相关系数大于0.998。该方法检出限(S/N>3)为0.05μg/kg,方法定量限(S/N>10)为0.3μg/kg,在0.3、1.0和2.0μg/kg 3个添加水平下的回收率为80.2%~105.2%,相对标准偏差均小于8%(n=6)。结论本方法快速、灵敏、准确,适用于日常大批量蜂蜡样品中痕量氯霉素残留量的分析。Objective To establish a method for the determination of trace chloramphenicol residue in beeswax by n-hexane pretreatment-solid-phase extraction and high performance liquid chromatography-tandem mass spectrometry(SPE-HPLC-MS/MS). Methods The samples were predissolved with n-hexane and then extracted with water, purified by hydrophilic-lipophilic-balance(HLB)solid phase extraction cartridge, separated with Accucore XL C18 column, detected by multiple reaction monitoring(MRM) mode tandem mass spectrometry, and quantified by internal standard method. Results Chloramphenicol had a good linear relationship with peak area in the range of 0.3~10 ng/mL, and the correlation coefficient was greater than 0.998. The limits of detection(S/N>3) for chloramphenicol was 0.05 μg/kg, and the limits of quantification(S/N>10) was 0.3 μg/kg. The recoveries at the three addition levels of 0.3, 1.0 and 2.0 μg/kg were 80.2%~105.2%, and the relative standard deviations were all less than8%(n=6). Conclusion This method is rapid, sensitive and accurate. It is suitable for the determination of chloramphenicol residue in large quantities of beeswax samples.

关 键 词：固相萃取净化 高效液相色谱-串联质谱法 蜂蜡 氯霉素 

分 类 号：S896.2[农业科学—特种经济动物饲养] O657.63[农业科学—畜牧兽医]