直接提取-超高压液相色谱-电喷雾串联质谱法检测原料奶及奶制品中的四环素类抗生素

Determination of tetracycline antibiotics residues in milk and dairy products by direct extraction-UPLC-ESI-MS/MS

中文关键词:  四环素族  直接提取  超高压液相色谱-串联质谱法  奶  奶制品

英文关键词:tetracycline antibiotics  direct extraction  ultra pressure liquid chromatography-electrospray tandem mass spectrometry (UPLC-ESI-MS/MS)  milk  dairy products

中文摘要:

      目的 建立直接提取-超高压液相色谱-电喷雾串联质谱法(UPLC-ESIMS/MS)同时测定原料奶及奶粉中土霉素、四环素、金霉素、强力霉素4种四环素类药物的分析方法。方法 原料奶及奶粉样品经少量高氯酸沉淀蛋白、低温冷冻除脂后, 用C18色谱柱分离, 以0.1%甲酸水和乙腈为流动相进行梯度洗脱, 电喷雾串联质谱正离子模式扫描, 多反应监测模式(MRM)检测, 外标法定量。结果 4种四环素族药物在1~1000 ng/mL浓度范围内线性关系良好, 相关系数r均在0.993以上。本方法的定量限为(S/N≥10)为原料奶5μg/kg, 奶粉25 μg/kg, 在10、50、100 μg/kg三个加标水平下, 加标回收率为73.4%~99.4%, 相对标准偏差为0.8%~14.3%(n≥6)。结论 该方法简便快速、灵敏可靠、经济有效, 适用于原料奶及奶粉中土霉素、四环素、金霉素和强力霉素4种四环素族药物残留的测定。

英文摘要:

      Objective A method for the simultaneous determination of oxytetracycline, tetracycline, chlortetracycline, and doxycycline residues in milk and dairy products was developed using direct extraction and ultra pressure liquid chromatography-electrospray tandem mass spectrometry (UPLC-ESI-MS/MS). Methods Samples were extracted with little perchloric acid to precipitate protein and remove Frozen grease, separated by C18 column with gradient elution using acetonitrile and water (containing 0.1％ formic acid) and analyzed by UPLC-ESI-MS/MS under the positive mode using multiple reaction monitoring (MRM). The samples were quantified with external standard method. Results The method showed a good linearity over the range of 1~1000 ng/mL for 4 compounds of tetracycline antibiotics residue with r≥0.993. The detection limit (S/N≥10) of milk was 5 μg/kg , and that of dairy products was 25 μg/kg. The recoveries were 73.4%~99.4% at the spiked level of 10, 50 μg/kg, and 100 μg/kg with relative standard deviation of 0.8%~14.3%(n≥6). Conclusion This method is simple, accurate and reproducible, and it is suitable for the rapid analysis of tetracycline antibiotics in milk and dairy products.