液相色谱-串联质谱法同时测定蜂蜜中的林可霉素、甲硝唑和氯霉素

Simultaneous determination of lincomycin, metronidazole and chloramphenicol in honey by liquid chromatography-tandem mass spectrometry

中文关键词:  蜂蜜  林可霉素  氯霉素  甲硝唑  液相色谱-串联质谱法

英文关键词:honey  lincomycin  chloramphenicol  metronidazole  liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立液相色谱-串联质谱法同时检测蜂蜜中林可霉素、甲硝唑和氯霉素含量的分析方法。方法 蜂蜜样品加水溶解后, 过聚合物基质反相固相萃取柱净化, 经5%甲醇水溶液淋洗小柱, 再用70%甲醇水溶液洗脱目标化合物。采用0.1%甲酸水溶液和乙腈作为液相色谱流动相进行梯度洗脱。经多反应监测模式, 在正离子电离模式下测定甲硝唑和林可霉素, 在负离子电离模式下测定氯霉素。同位素稀释内标法定量。结果 本方法在10 min内通过质谱正负离子电离模式切换对林可霉素、甲硝唑和氯霉素进行同时测定。3个目标化合物在0.25、5和25 μg/kg添加水平的回收率为91.0%~107.1%, 相对标准偏差小于11.9%(n=6), 林可霉素、甲硝唑和氯霉素的方法定量限分别为0.20、0.14和0.20 μg/kg。结论 本方法易于操作, 灵敏度和重现性良好, 适用于监督抽检和风险监测等大批量检测工作。

英文摘要:

      Objective To establish an analytical method for the simultaneous determination of lincomycin, metronidazole and chloramphenicol in honey by liquid chromatography-tandem mass spectrometry. Methods Honey samples were diluted with water. And then a polymer reversed phase solid phase extraction cartridge was used to purify the sample. The cartridge was rinsed with 5% methanol aqueous solution and subsequently the target compounds were eluted by 70% methanol aqueous solution. The chromatography separation was carried out with a gradient elution program consisted of 0.1% formic acid aqueous solution and acetonitrile as mobile phases. With multiple reactions monitoring, lincomycin and metronidazole were identified under positive ionization mode, while chloramphenicol was analyzed under positive ionization mode. Quantitation was done by isotope dilution internal standard method. Results The simultaneous determination of lincomycin, metronidazole and chloramphenicol was achieved within 10 mins, using positive/negative switched ionization mode. The recoveries were ranged from 91.0% to 107.1% for the analytes with 3 spiked levels of 0.25, 5 and 25 μg/kg. The relative standard deviations were less than 11.9% (n=6), and the limits of quantitation for lincomycin, metronidazole and chloramphenicol were 0.20, 0.14 and 0.20 μg/kg, respectively. Conclusion The proposed method is easy, sensitive and well-reproduced, which is suitable for massive sample analysis such as risk monitoring.