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同时测定自来水中27种抗生素残留全自动固相萃取-超高效液相色谱-串联质谱法建立

Simultaneous determination of antibiotics in tap water with automatic solid phase extraction-UHPLC-MS/MS

  • 摘要:
      目的  建立一种同时检测自来水中四环素类、大环内酯类、氟喹诺酮类、酚类和磺胺类27种抗生素残留的全自动固相萃取 – 超高效液相色谱 – 串联质谱分析方法。
      方法  采集200 mL自来水样本在24 h内加入内标混合溶液,经玻璃纤维滤纸过滤后,调节pH到7.5~8.5;在全自动固相萃取仪上使用固相萃取柱完成样本富集,用甲醇溶液洗脱后氮吹至干,20 %甲醇水溶液复容,经T3色谱柱在40 %乙腈甲醇 – 0.2 %甲酸水溶液的流动相下梯度分离,高效液相色谱串联质谱检测,内标法定量分析;并采用该方法对浙江省某农村地区的70份自来水样本进行检测。
      结果  实验结果显示,27种抗生素在1~100 ng/mL范围内线性关系良好,r值为0.9963~1.0000;该方法检出限(MDL)为0.004~0.296 ng/L,方法定量限(MQL)为0.013~0.988 ng/L,平均回收率为70.0 %~120.8 %;通过对浙江省某农村70份自来水样本进行检测,检测到4种抗生素残留,皆为大环内酯类抗生素,分别为罗红霉素(0.162~2.858)ng/L、克拉霉素(0.063~0.849)ng/L、红霉素(0.100~1.804)ng/L和替米考星(0.167~1.418)ng/L,其余23种抗生素均未检出。
      结论  本研究建立的全自动固相萃取 – 超高效液相色谱 – 串联质谱法操作简单、省时省力、灵敏度高、准确可靠,可适用于自来水中27种抗生素残留的快速检测。

     

    Abstract:
      Objective  To establish a rapid method for simultaneous determination of 27 antibiotics in tap water with ultra high performance liquid chromatography with tandem mass spectrometry (UHPLC-MS/MS) combined with automatic solid phase extraction.
      Methods   After added internal standard solutions of 27 antibiotics within 24 hours, the tap water sample (200 mL) was filtered with glass fiber filters and adjusted for pH value of 7.5 – 8.5. The reference antibiotics in the tap water samples were concentrated with extraction column in the automated solid phase extraction instrument and then eluted with methanol solution. The reference antibiotics in the eluate was reconstituted into constant solution with 20% methanol and separated gradiently with T3 chromatography column using 40% acetonitrile methanol and 0.2% formic acid solution as mobile phase; and finally detected with UHPLC-MS/MS and quantified with internal standard method. Thereafter, 70 tap water samples were collected in rural areas of Zhejiang province and 27 antibiotics in the samples were detected simultaneously using the established method.
      Results  A good linearity was observed for detections of the 27 antibiotics at the concentration of 1 to 100 ng/mL, with the correlation coefficient ranging from 0.9963 to 1.0000. For the established method, the detection limits were between 0.004 – 0.296 ng/L; the quantification limits were from 0.013 to 0.998 ng/L; and the mean recoveries ranged from 70.0% – 120.8%. For the 70 rural tap water samples, only four macrolide antibiotics were detected, including roxithromycin, clarithromycin, erythromycin, and tilmicosin, with the concentration ranges (ng/L) of 0.162 – 2.858, 0.063 – 0.849, 0.100 – 1.804, and 0.100 – 1.804, respectively.
      Conclusion   The established method is simple to operate, time- and labor-saving; the method is also of high sensitivity, accuracy and reliability; and the method could be applied to rapid determination of 27 antibiotics in tap water.

     

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