基于全羟基取代六元瓜环的固相微萃取搅拌棒对环境水样中非甾体抗炎药物的分析检测

发布时间：2018-11-09 17:00

【摘要】：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。
[Abstract]:Objective: to establish a method for simultaneous determination of four non-steroidal anti-inflammatory drugs ibuprofen, meloxicam, naproxen and naproxen in environmental water by solid-phase microextraction (SPME) agitator (SBSE) and high performance liquid chromatography (HPLC) based on total hydroxyl substituted six-component melon ring. Method for determination of diclofenac sodium. Methods: 5 mL water samples were enriched by solid phase microextraction with {(OH) _ (12) Q [6]} derivative and extracted by self-made total hydroxyl groups instead of hexagonal melons. The extraction rods were analyzed by methanol 200 渭 L ultrasonic analysis, and methanol 20 渭 L was extracted by HPLC. Using C18 column as analytical column, methanol-20 mmol L ~ (-1) ammonium acetate (containing 0.1% acetic acid) (70:30) as mobile phase, flow rate 1.0 mL min~ (-1), UV 270 nm). Results: the linear range of meloxicam, naproxen and diclofenac sodium was 10 ~ 2 500 渭 g / L ~ (-1), and the linear range of ibuprofen was over 0.997 渭 g / L ~ (-1). The detection limit of the four drugs was within the range of 0.7 渭 g / L ~ (-1). The average recovery rate (nu _ 3) of the two concentration levels was in the range of 90.5 渭 g / L ~ (-1), and the RSD was lower than 9.8% in the range of 90.5 渭 g / L ~ (-1). Four NSAIDs were not detected in wastewater from Huaxi River and Jinyang sewage. Conclusion: this method can be used for the determination of trace non-steroidal anti-inflammatory drugs in environmental water samples.
【作者单位】：贵州大学化学与化工学院;
【基金】：国家自然科学基金项目(81160398,21665005) 贵州大学研究生创新基金(研理工2017001)
【分类号】：R917

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