摘要
目的建立同位素稀释液相色谱-串联质谱法测定禽肉、禽蛋中地克珠利、尼卡巴嗪、托曲珠利和托曲珠利砜4种抗球虫药含量的方法。方法用多种溶剂分别提取抗球虫药,同时加入同位素内标液,内标法测定,比较各提取液的回收率。采用多种流动相种类、比例和洗脱持续时间测定,选择最佳流动相条件和梯度洗脱程序,在质谱直接进样模式下进行质谱条件优化。在优化条件下,进行检出限、回收率测定等方法学评价实验。结果采用甲醇∶乙腈(1∶1)作为提取剂,0.03%甲酸溶液和甲醇作为流动相,C18色谱柱(100 mm×2.1 mm,1.7μm),在0.5~10.0μg/L浓度范围内相关系数r≥0.999,加标回收率为75.0%~102.1%,方法的检出限为0.11~0.20 mg/kg。结论该方法前处理较简捷,准确性及精密度高,线性范围较广。与国标方法及现行其他方法相比,检出限、准确度及精密度均符合要求,适合基层大批样品的抗球虫药含量检测。
Objective To establish an isotope dilution liquid chromatography-tandem mass spectrometry method for the determination of four-anticoccidial-drug contents in poultry and eggs,namely diclazuli,nicardipine,toclazuli,and toclazuli sulfone.Methods Multiple solvents were used to extract anti-coccidiosis drugs,and isotopic internal standard solutions were added.The internal standard method was used to determine,and the recovery rates of various extraction solutions were compared.Multiple types,ratios,and elution durations of mobile phases were used for determination,and the optimal mobile phase conditions and gradient elution program were selected.Mass spectrometry conditions were optimized in direct injection mode.Methodological evaluation experiments including detection limit and recovery rate determination were conducted under optimized conditions.Results The solution with methanol∶acetonitrile(1∶1)was used as the extraction agent;0.03%formic acid solution and methanol were used as the mobile phase;C18chromatographic column(100 mm×2.1 mm,1.7μm)was employed;the correlation coefficient r was≥0.999 in the concentration range of 0.5-10.0μg/L.The recovery rate was between 75.0%-102.1%,and the detection limit of the method were between 0.11-0.20 mg/kg.Conclusions The method has simple pre-treatment,high accuracy and sensitivity,and a wide linear range.Compared with the national standard method and other current methods,the detection limit,accuracy,and precision all met the requirements,it is suitable for detecting the content of anti coccidian drugs at the grassroots level.
作者
谢莉
张清杰
赵俊君
XIE Li;ZHANG Qingjie;ZHAO Junjun(Puyang Center For Disease Control and Prevention,Puyang,Henan 457000,China)
出处
《现代疾病预防控制》
2025年第2期154-158,共5页
MODERN DISEASE CONTROL AND PREVENTION
关键词
同位素稀释
液相色谱-串联质谱
抗球虫药
固相萃取
Isotope dilution
Liquid chromatography-tandem mass spectrometry
Anticoccidial drug:Solid phase extraction
