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

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 mL环境水样经用自制的全羟基取代六元瓜环{（OH）₁₂Q[6]}衍生的固相微萃取搅拌棒萃取富集，萃取小棒经甲醇200 μL超声解析后，取甲醇20 μL进样HPLC测定。采用C₁₈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 mL·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10~2 500 μg·L^-1，布洛芬的线性范围在100~10 000 μg·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 homemade stir bar sorptive extraction (SBSE) coupled with HPLC for simultaneous determination of 4 kinds of non-steroid anti-inflammatory drugs ibuprofen, meloxicam, naproxen and diclofenac sodium.Methods: 5 mL environmental water sample was extracted by homemade microextraction stir bar based on perhydroxy cucurbit[6]uril {(OH)₁₂Q[6]}.After extraction, the stir bar was placed in a glass desorption tube containing 200 μL of methanol and was treated in an ultrasonic bath.A 20 μL volume of desorption solution was injected into the HPLC-UV instrument for subsequent analysis.Isocratic separation was carried out using a reversed-phase C₁₈ column and a mobile-phase flow rate of 1.0 mL·min^-1, with UV detection at 270 nm.The mobile phase used consisted of 70% methanol in water and 20 mmol·L^-1 ammonium acetate solution (containing 0.1% acetic acid) (70:30).Results: The linear range is from 10 to 2 500 μg·L^-1 for meloxicam, naproxen and diclofenac sodium and 100-10 000 μg·L^-1 for ibuprofen with the correlation coefficients above 0.997 2.The detection limits of 4 drugs ranged between 0.7-40.3μg·L^-1.The average recoveries (n=3) were in the range of 90.5%-115.8% at two spiked levels, and the relative standard deviations were less than 9.8%.4 kinds of non-steroid anti-inflammatory drugs were not detected in the Huaxi river and wastewater samples of Jinyang sewage treatment plant.Conclusion: The established method is proved by methodology validation, which is suitable for the determination of trace non-steroid anti-inflammatory drugs in environmental water samples.