| 高效液相色谱-串联质谱法测定蜂蜜中氯霉素、甲砜霉素、氟甲砜霉素及甲硝唑 |
| |
| 引用本文： | 李潇舟,陈海平.高效液相色谱-串联质谱法测定蜂蜜中氯霉素、甲砜霉素、氟甲砜霉素及甲硝唑[J].现代预防医学,2022,0(13):2420-2425. |
| |
| 作者姓名： | 李潇舟 陈海平 |
| |
| 作者单位： | 北京市海淀区疾病预防控制中心，北京 100094 |
| |
| 摘 要： | 目的 建立蜂蜜中氯霉素、甲砜霉素、氟甲砜霉素及甲硝唑残留的高效液相色谱-串联质谱同时测定方法。方法 以乙酸乙酯作为提取剂，经涡旋混匀提取后，氮吹至干，用5%甲醇水溶解，Oasis HLB固相萃取柱净化。经甲醇洗脱，洗脱液经45℃水浴氮吹至干，流动相涡旋溶解，上机测定。高效液相色谱分离、串联质谱检测，采用多离子反应监测（MRM）模式，内标法定量。结果 在优化条件下，4种抗生素浓度在0.1～5.0μg/L范围内，线性关系良好，相关系数（r）≥0.9953，方法检出限≤0.015μg/kg，不同基质中平均加标回收率为78.5%～95.1%，相对标准偏差（RSD）为2.8%～10.7%。结论 该方法快速、灵敏、准确，适用于蜂蜜中氯霉素、甲砜霉素、氟甲砜霉素及甲硝唑的同时测定。
|
| 关 键 词： | 抗生素 蜂蜜 固相萃取 高效液相色谱-串联质谱法 |
Determination of residues of chloramphenicol,thiamphenicol, florfenicol and metronidazole in Honey by HPLC-MS/MS |
| |
| LI Xiao-zhou,CHEN Hai-ping.Determination of residues of chloramphenicol,thiamphenicol, florfenicol and metronidazole in Honey by HPLC-MS/MS[J].Modern Preventive Medicine,2022,0(13):2420-2425. |
| |
| Authors: | LI Xiao-zhou CHEN Hai-ping |
| |
| Affiliation: | Haidian District Center for Disease Control and Prevention, Beijing 100094, China |
| |
| Abstract: | Objective To establish a method for simultaneous determination of chloramphenicol, thiamphenicol, florfenicol and metronidazole residues in honey by high-performance liquid chromatography-tandem mass spectrometric method (HPLC-MS/MS). Methods The residue was extracted by vortex mixing, which used ethyl acetate as extractant, then dried-up under nitrogen flow, and dissolved in 5% methanol-water. The sample solution was purified with Oasis HLB solid phase extraction column. After elution with methanol, the eluent was blown to dryness under nitrogen flow in water bath at 45℃. The residue was dissolved in mobile phase by vortex, and separated by using HPLC and detected by MS / MS in positive and negative ion multiple reaction monitoring (MRM) mode. The quantifications were based on internal standard method. Results Under the optimized conditions, the calibration curves for the 4 antibiotics were linear in the range of 0.1-5.0μg/L with the correlation coefficients (r) of ≥ 0.9953, and the limit of detection was 0.015 μg/kg. The average recovery rates of 4 antibiotics residues from different matrices were within 78.5％-95.1％, and the relative standard deviations (RSD) range were 2.8%-10.7%. Conclusion The method is effective, sensitive, and accurate. It can be used to simultaneously determine the residues of chloramphenicol, thiamphenicol, florfenicol and metronidazole in honey. |
| |
| Keywords: | Antibiotic Honey Solid phase extraction High-performance liquid chromatography/mass spectrometry (HPLC-MS/MS) |
|
| 点击此处可从《现代预防医学》浏览原始摘要信息 |
|
点击此处可从《现代预防医学》下载全文 |
|
