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| UPLC-MS/MS高通量测定鸡粪中81种抗菌药物残留方法的建立 |
| UPLC-MS/MS Sample pretreatment methods for high-throughput determination of 4 groups of 81 antimicrobial residues in chicken manure |
| 投稿时间：2024-02-28 修订日期：2024-04-25 |
| DOI： |
| 中文关键词: 鸡粪 超高效液相色谱-串联质谱法 抗菌药物 残留 |
| 英文关键词: chicken manure ultra performance liquid chromatography-tandem mass spectrometry antimicrobial drug residues |
| 基金项目:中国动物卫生与流行病学中心创新(2021221200) |
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| 中文摘要: |
| (目的)本方法通过比较、优化样品前处理方法,建立了一种超高效液相色谱-串联质谱法(UPLC-MS/MS)高通量、快速测定鸡粪中磺胺类、大环内酯类、喹诺酮类、四环素类等4类81种抗菌药物残留检测方法。(方法)准确称取2.00 g经冻干、研磨处理的鸡粪样品,加入20 mL体积比为5:15(v/v)的EDTA-Mcllvaine与乙腈/乙酸混合溶液,超声15 min,涡动提取15 min,上清液45℃水浴氮吹后用EDTA-Mcllvaine缓冲液复溶；HLB固相萃取柱净化过柱后,依次用3 mL水和3 mL 5%甲醇淋洗,最后以3 mL 5%的氨化甲醇洗脱,洗脱液氮吹后用1 mL 0.1%甲酸水/乙腈充分溶解并定容,0.22 μm滤膜过滤后上机检测。(结果)加标回收试验结果显示,鸡粪中81种药物在1.0～100 μg kg－1范围内线性关系良好(R2>0.99),检出限为1.0～2.5 μg kg－1,待测药物的回收率为60.24%～118.70%。(结论)该方法简单可靠,提取效果好,适用于鸡粪中多类抗菌药物残留的大批样品筛查和确证。 |
| 英文摘要: |
| By comparing and optimizing the sample pretreatment methods, an ultra-high performance liquid chromatogram-tandem mass spectrometry (UPLC-MS/MS) method was established for the rapid and high throughput determination of 81 antimicrobial drug residues in chicken feces, including 4 types of sulfonamides, macrolides, quinolones and tetracycline. 2.00g freeze-dried and ground chicken manure samples were accurately weighed, and 20 mL EDTA-Mcllvaine mixed with acetonitrile/acetic acid with a volume ratio of 5:15(v/v) was added. The samples were extracted by ultrasonic for 15 min and eddy for 15 min. The supernatant was redissolved with EDTA-Mcllvaine buffer after blowing nitrogen in water bath at 45℃. After the HLB solid phase extraction column was purified, the column was washed with 3 mL water and 3 mL 5% methanol in sequence, and finally eluted with 3 mL 5% ammoniated methanol. After blowing the elution liquid nitrogen, the elution liquid was fully dissolved with 1 mL 0.1% formic acid water/acetonitrile and fixed volume, and then filtered by 0.22 μm filter membrane, the column was tested by machine. The standard recovery test showed that the linear relationship of 81 drugs in chicken feces was good in the range of 1.0 ~ 100 μg kg－1 (R2>0.99), the detection limit was 1.0 ~ 2.5 μg kg－1, and the recovery rate was 60.24% ~ 118.70%.The method is simple, reliable and has good extraction effect. It is suitable for screening and confirming the residues of many kinds of antibiotics in chicken manure. |
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