地表水中10种抗生素SPE-HPLC-MS/MS检测方法的建立
Simultaneous determination of 10 antibiotic residues in surface water by SPE-HPLC-MS/MS
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摘要: 应用固相萃取（SPE）-高效液相色谱-串联三重四极杆质谱（HPLC-MS/MS）技术，建立了地表水中10种抗生素（甲氧苄啶、氨苄西林、头孢氨苄、头孢噻肟钠、红霉胺、罗红霉素、螺旋霉素、磺胺甲恶唑、克拉霉素、夫西地酸钠）的分析检测方法.水样经过HLB小柱浓缩萃取之后，以反相色谱柱Shim-pack XR-ODS为分析柱，乙腈和0.1%甲酸-水溶液为流动相，采用HPLC-MS/MS多反应监测（MRM）离子模式进行分析.结果表明，所建立方法的方法检出限（MDL）为0.0056—3.9675 ng·L-1，基质加标回收率为50%—127%，平行样品间相对标准偏差均小于11% （n = 6）.该方法操作简单、定性定量准确，检出限低，能够满足测定地表水环境中抗生素痕量残留的分析要求.应用该方法测定了北京地区清河地表水中上述10种抗生素的残留状况.
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关键词:
- 抗生素 /
- 固相萃取 /
- 高效液相色谱-串联质谱 /
- 地表水 /
- 新兴污染物
Abstract: A rapid analytical method for the determination of ten antibiotics including trimethoprim,ampicillin,cephalexin,cefotaxime sodium,erythromycylamine,roxithromycin,spiramycin,sulfamethoxazole,clarithromycin,and sodium fusidate in surface water was established by using solid phase extraction (SPE) and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Samples were passed through HLB cartridges in order to extract and purify the antibiotics from surface water samples. The targeted antibiotics were separated on a Shim-pack XR-ODS column using water with 0.1% formic acid and acetonitrile (V∶V) as the mobile phase. The antibiotics were quantified under multiple reaction monitoring (MRM) mode. The method detection limits (MDLs) were 0.0056—3.9675 ng·L-1. The recovery rates were 50%—127%, and the relative standard deviations between samples were all below 11% (n = 6). The developed method could meet the need for the detection of antibiotics in surface water samples, because it is simple and accurate, and has low MDLs. The method was applied to the determination of the ten antibiotics in surface water from Qinghe River in Beijing. -
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