Simultaneous determination of metronidazole, chloramphenicol and 10 sulfonamide residues in honey by LC-MS/MS
Simultaneous determination of metronidazole, chloramphenicol and 10 sulfonamide residues in honey by LC-MS/MS
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DOI：
10.1039/c2ay25998b
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发表时间：
2013-01-01
影响因子：
3.1
通讯作者：
Chen, Zhongzhou
中科院分区：
文献类型：
--
作者：
Tian, Wenli;Gao, Lingyu;Chen, Zhongzhou
建立了同时测定蜂蜜中甲硝唑、氯霉素和磺胺类10种磺胺类药物(磺胺类、磺胺类)残留量的高效液相色谱-串联质谱法。样品首先溶解在水中。在超声浴中用乙腈超声提取目标分析物，并用旋转蒸发浓缩。色谱柱为MGIII-C-18柱(2.1 mm×150 mm，5µm)，流动相为甲醇-50 mm L-1醋酸铵水溶液(含0.3%甲酸)，梯度洗脱。采用阴离子或阳离子选择性反应监测模式对甲硝唑、氯霉素和磺胺类药物进行监测，并采用外标法进行定量。氯霉素的检出限为0.1mgkg-1，甲硝唑和磺胺的检出限分别为1.0mgkg-1。氯霉素、甲硝唑和磺胺类药物的线性范围分别为0.10~25.0mgkg(-1)和1.0~100.0 mgkg(-1)，相关系数均大于0.99。方法的平均加标回收率为81.6%~99.7%，相对标准偏差为3.61~8.97%。该方法简便、快速、灵敏、可靠，可用于商品中甲硝唑、氯霉素和10种磺胺类药物残留量的同时检测。
A liquid chromatography-tandem mass spectrometric method was established for the simultaneous determination of residues of metronidazole, chloramphenicol and 10 sulfonamides (sulfadiazine, sulfathiazol, sulfapyridin, sulfamerazin, sulfameter, sulfamethazine, sulfamethoxypyridazine, sulfachloropyridazine, sulfamethoxazole and sulfadimethoxin) in honey samples. Samples were first dissolved in water. Sonication was carried out in an ultrasonic bath to extract the target analytes with acetonitrile and the extract was concentrated by rotary evaporation. Chromatographic separation was carried out on an MGIII-C-18 column (2.1 mm x 150 mm, 5 mu m) using a mobile phase made up of methanol and 50 mmol L-1 ammonium acetate aqueous solution (include 0.3% formic acid) and gradient elution. Metronidazole, chloramphenicol and the sulfonamides were monitored in negative ion or positive ion selected reaction monitoring modes and quantified by the external standard method. The limit of detection was 0.1 mu g kg(-1) for chloramphenicol and 1.0 mu g kg(-1) for metronidazole and each sulfonamide, respectively. The linear range for chloramphenicol was 0.1-25.0 mu g kg(-1), and for both metronidazole and the sulfonamides were 1.0-100.0 mu g kg(-1), and all the correlation coefficients were greater than 0.99. The average spike recoveries of the method ranged from 81.6% to 99.7% with relative standard deviations of 3.61-8.97%. Therefore this method is convenient, rapid, sensitive and reliable, and can be successfully applied for the simultaneous detection of metronidazole, chloramphenicol and 10 sulfonamide residues in commercial products.