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    超声提取-凝胶渗透色谱法净化-超高效液相色谱-串联质谱法测定鸭肠及其制品中6种常见抗生素的残留量

    Determination of 6 Common Antibiotics Residues in Duck Intestine and Its Products by UHPLC-MS/MS after Ultrasonic Extraction and GPC Purification

    • 摘要: 建立了超声提取-凝胶渗透色谱法(GPC)净化-超高效液相色谱-串联质谱法(UHPLC-MS/MS)测定鸭肠及其制品中6种常见抗生素残留量的分析方法。将鸭肠或鸭肠制品粉碎后,取样品12.0 g至50 mL塑料离心管中,依次加入甲醇30 mL、氨水1.0 mL、除水剂无水硫酸钠3.0 g,均质1 min,超声提取15 min,冷冻离心6 min,上清液全部转移至GPC净化瓶中,按GPC条件进行净化处理,将收集的淋洗液用氮吹仪氮吹至近干,残渣加1 mL甲醇溶解,经0.45 μm滤膜过滤,滤液采用UHPLC-MS/MS定性、定量检测。结果显示:替米考星、罗红霉素、红霉素、氧氟沙星、环丙沙星、氟苯尼考的质量浓度在0.01~10.00 mg·L-1内与对应的峰面积呈线性关系,检出限(3S/N)依次为0.221,0.153,0.396,0.112,0.577,0.089 μg·kg-1。按标准加入法进行回收试验,回收率为82.4%~107%,测定值的相对标准偏差(n=6)均小于5.0%。

       

      Abstract: A method was established for the determination of 6 common antibiotic residues in duck intestine and its products by ultra high pressure liquid chromatography triple quadrupole-mass spectrometry (UHPLC-MS/MS) after ultrasonic extraction and gel permeation chromatography (GPC) purification. The samples (12.0 g) were placed into a 50 mL plastic centrifuge tube after the duck intestines or its products were crushed, and 30 mL of methanol, 1.0 mL of ammonia water and 3.0 g of anhydrous sodium sulfate as dehydrant were followed. The samples were homogenized for 1 min, extracted by ultrasonic for 15 min, and refrigerated for 6 min. The supernatant was all transferred to the GPC purification bottle and purified under the GPC conditions. The collected eluent was put into a nitrogen blower and blown to nearly dryness by nitrogen. The residue was dissolved with 1 mL of methanol and filtered through a 0.45 μm membrane. The filtrate was qualitatively and quantitatively detected by UHPLC-MS/MS. The results showed that linear relationships between values of peak area and mass concentration of temicocacin, roxithromycin, erythromycin, ofloxacin, ciprofloxacin and florfenicol were found in the range of 0.01-10.00 mg·L-1, with detection limits (3S/N) of 0.221, 0.153, 0.396, 0.112, 0.577, 0.089 μg·kg-1, respectively. Test for recovery was made by standard addition method, giving results in the range of 82.4%-107%, with RSDs (n=6) of the determined values less than 5.0%.

       

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