固相萃取-超高效液相色谱法测定饮用水中四环素类抗生素
Determination of Tetracyclines in Drinking Water by Ultra High Performance Liquid Chromatography Coupled with Solid Phase Extraction
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摘要:
目的 建立一种固相萃取-超高效液相色谱测定饮用水中四环素类抗生素的检测方法。
方法 取200 mL水样，以10～15 mL/min的流速通过Oasis HLB固相萃取小柱，然后用甲醇和乙酸乙酯混合溶液（体积比为1∶9）洗脱，氮气吹干，以体积分数为30%的甲醇溶液定容至1.0 mL，取10 μL水样采用超高效液相色谱仪进行检测。
结果 4种抗生素的线性范围为0.05～1.00 mg/L，
r >0.998，方法检出限为0.063～0.250 μg/L，方法的平均加标回收率为77.2%～136.0%，相对标准偏差为0.88%～5.86%。12份出厂水和末梢水均未检出目标抗生素。结论 本方法样品前处理简便、液相色谱分析时间短、线性范围宽、检出限较低，适合检测饮用水中四环素类抗生素。
Abstract:Objective To build a method to determine tetracyclines in drinking water by ultra high performance liquid chromatography (UPLC) coupled with solid phase extraction.
Methods Water sample (200 mL) was added to Oasis HLB solid phase extraction column at 10-15 mL/min, then eluted by methanol and ethylacetate mixture (v/v, 1:9), dried with nitrogen, and dissolved to the mark of 1.0 mL using 30% methanol solution. Then 10 μL final processed sample was injected in UPLC.
Results The standard curves for the four tetracyclines were linear over the concentration range of 0.05-1.00 mg/L, with correlation coefficients all above 0.998. The limits of detection were 0.063-0.250 μg/L. The average recoveries ranged from 77.2% to 136.0%, and the relative standard deviations were in the range of 0.88% to 5.86%. No selected tetracyclines were detected in 12 samples of treated water and tap water.
Conclusion This method has advantages of simple pre-treatment, rapid UPLC analysis, wide linear range, and low limits of detection, so it can be used to detect tetracyclines in drinking water.
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