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目的:建立基于全羟基取代六元瓜环的自制固相微萃取搅拌棒(SBSE)-高效液相色谱(HPLC)联用同时测定环境水样中4种非甾体抗炎药物布洛芬,美洛昔康,萘普生,双氯芬酸钠的分析测定方法。方法:5 m L环境水样经用自制的全羟基取代六元瓜环{(OH)_(12)Q[6]}衍生的固相微萃取搅拌棒萃取富集,萃取小棒经甲醇200μL超声解析后,取甲醇20μL进样HPLC测定。采用C_(18)柱为分析柱,甲醇-20 mmol·L~(-1)乙酸铵(含0.1%乙酸)(70∶30)为流动相,流速1.0 m L·min~(-1),UV 270 nm波长处进行检测。结果:美洛昔康,萘普生,双氯芬酸钠线性范围为10~2 500μg·L~(-1),布洛芬的线性范围在100~10 000μg·L~(-1)之间,相关系数均大于0.997 2;4个药物的检测限在0.7~40.3μg·L~(-1)范围内,2个浓度水平平均回收率(n=3)在90.5%~115.8%范围内,RSD低于9.8%;花溪河水和金阳污水产的污水未检测出4个非甾体药物。结论:本法经方法学验证可用于环境水样中痕量非甾体抗炎药物的分析检测。
OBJECTIVE: To establish a home-made solid-phase microextraction (SBSE) -high performance liquid chromatography (HPLC) combined with all-hydroxyl-substituted six-membered melon rings for the simultaneous determination of four nonsteroidal antiinflammatory drugs, ibuprofen, Meloxicam, naproxen, diclofenac sodium analysis and determination methods. Methods: The 5 m L environmental water samples were extracted with a solid phase microextraction stirrer rod derived from the all-hydroxyl-substituted 6-membered guaiac {{OH) _ (12) Q [6]}. After sonication, 20 μL methanol was injected into the HPLC. The mobile phase consisted of C_ (18) column, methanol-20 mmol·L -1 ammonium acetate (containing 0.1% acetic acid) (70:30) and the flow rate was 1.0 m L · min -1. UV 270 nm wavelength detection. Results: The linear range of meloxicam, naproxen and diclofenac sodium was 10-2 500 μg · L -1, and the linear range of ibuprofen was between 100 and 10 000 μg · L -1 The detection limits of four drugs ranged from 0.7 to 40.3 μg · L -1, and the average recoveries of two concentration levels (n = 3) ranged from 90.5% to 115.8% At 9.8%; 4 non-steroidal drugs were not detected in the sewage of Huaxi River and Jinyang Sewage. Conclusion: This method is validated by methodology for the analysis of trace NSAIDs in environmental water samples.