超声辅助离子液体液相微萃取-高效液相色谱法分析水样中加替沙星或氟罗沙星

doi:10.3724/SP.J.1095.2014.30087

摘要/Abstract

摘要： 建立了一种采用离子液体1-己基-3-甲基咪唑六氟磷酸([C6mim][PF6])为萃取剂，超声辅助离子液体液相微萃取-高效液相色谱法分析水样中加替沙星和氟罗沙星的方法。实验考察了溶液酸度、离子液体用量等因素对萃取的影响。在pH值分别为3.3、2.1的加替沙星和氟罗沙星水样中，加入0.4 mL [C6mim][PF6]，超声，离心，离子液体相直接用于HPLC进行分析。该方法的线性范围为0.5~50 mg/L,测定加替沙星和氟罗沙星的相对标准偏差(n=5)为2.80%和5.93%,二者的检出限分别为0.46、0.97 μg/L，该方法萃取水样中加替沙星的加标回收率为80.5%~89.5%，氟罗沙星的加标回收率可达93.3%~99.0%。

关键词: 加替沙星, 氟罗沙星, 离子液体, 超声波

Abstract: A method was established for the analysis of gatifloxacin or fleroxacin in water sample by ultrasonic assisted hydrophobic ionic liquid (1-hexyl-3-methylimidazolium hexafluorophosphate, [C6mim][PF6]) liquid-phase microextraction coupled with high performance liquid chromatography(HPLC). The pH value of solution, amount of ionic liquid and other factors which might affect the extraction efficiency were researched. To gatifloxacin water sample at pH=3.3 and fleroxacin water sample at pH=2.1 was added 0.4 mL of [C6mim][PF6], respectively, for ultrasonic extraction. After extraction, phase separation was performed by centrifugation. The sediment phase were injected into the HPLC system for analysis. By this method, the linear ranges for analysis are 0.5~100 μg/L and the relative standard deviations(n=5) for them are 2.80 and 5.93, respectively. The limits of detection(3S/N) for gatifloxacin and fleroxacin are 0.46 and 0.97 μg/L, respectively. Under the above mentioned conditions, the extraction recoveries for gatifloxacin or fleroxacin water samples were found to be 80.5%~89.5% and 93.3%~99.0%, respectively.

Key words: gatifloxacin, fleroxacin, ionic liquid, ultrasounic extraction

中图分类号:

O658.2

张婧, 赵文岩, 刘富强, 王晓黎. 超声辅助离子液体液相微萃取-高效液相色谱法分析水样中加替沙星或氟罗沙星[J]. 应用化学, DOI: 10.3724/SP.J.1095.2014.30087.

ZHANG Jing, ZHAO Wenyan*, LIU Fuqiang, WANG Xiaoli. Determination of Gatifloxacin or Fleroxacin in Water Sample by Ultrasound-Assisted Ionic Liquid Liquid-Phase Microextraction Coupled with High Performance Liquid Chromatography[J]. Chinese Journal of Applied Chemistry, DOI: 10.3724/SP.J.1095.2014.30087.

参考文献

[1] ZHANG Yujie,LI Qian,WANG Xia,et al. Determination of Fluoroquinolones in Tissues of Several Animals by HPLC[J]. Chinese J Vet Drug,2012，46(7):65-68(in Chinese).

张玉洁，李倩，汪霞，等. 高效液相色谱法检测多种动物组织中氟喹诺酮类药物残留量的研究[J]. 中国兽药杂志，2012，46(7):65-68.

[2] YU Suhua,MENG Wenjing,LU Tingting,et al. Spectrophotometric, Spectrofluorimetric and Reversed-phase High-performance Liquid Chromatographic Methods for Determination of Gatifloxacin in Its Capsule[J]. J Yangzhou Univ(Nat Sci Edn),2008，11(2):40-44(in Chinese).

于素华，孟文静，陆婷婷，等. 加替沙星的紫外、荧光分光光度法和高效液相色谱法测定[J]. 扬州大学学报(自然科学版)，2008，11（2）：40-44.

[3] LI Sheng,YAO Junxue,AO DENG Gaowa. Spectrophot Ometric Study on Fleroxacin and Its Application[J]. J Inner Mongolia Univ(Nat Sci Edn),2005，36(3):273-275(in Chinese).

李胜,姚俊学,敖登高娃. 氟罗沙星的分光光度法研究及应用[J]. 内蒙古大学学报(自然科学版),2005，36(3):273-275.

[4] Han J,Wang Y,Yu C L. Extraction and Determination of Chloramphenicol in Feed Water, Milk, and Honey Samples Using an Ionic Liquid/Sodium Citrate Aqueous Two-phase System Coupled with High-performance Liquid Chromatography[J]. Anal Bioanal Chem,2011,399:1295-1304.

[5] Zhang Y F,Lee H. Ionic Liquid-based Ultrasound-assisted Dispersive Liquid liquid Microextraction Followed High-performance Liquid Chromatography for the Determination of Ultraviolet Filters in Environmental Water Samples[J]. Anal Chim Acta,2012,750:120-126.

[6] Han D D，Row K H. Determination of Luteolin and Apigenin in Celery Using Ultrasonic-assisted Extraction Based on Aqueous Solution of Ionic Liquid Coupled with HPLC Quantification[J]. J Sci Food Agric,2011,91:2888-2892.

[7] Ma C H,Wang S Y,Yang L,et al. Ionic Liquid-aqueous Solution Ultrasonic-assisted Extraction of Camptothecin and 10-Hydroxycamptothecin from Camptotheca Acuminata Samara[J]. Chem Eng Proc，2012，57:59-64.

[8] Lou Z X,Wang H X,Zhu S,et al. Ionic Liquids Based Simultaneous Ultrasonic and Microwave Assisted Extraction of Phenolic Compounds from Burdock Leaves[J]. Anal Chim Acta,2012,716:28-33.

[9] LIU Meihua,QIU Bin,CHEN Guonan,et al. Determ Ination of Estrogens in Waste Water by Ultrasound-Assisted Ionic Liquid Dispersive Liquid-Phase Microextraction Coupled with High Performance Liquid Chromatography[J]. Anal Test Technol Instrum,2009,15(3):151-157(in Chinese).

刘美华,邱彬,陈国南,等. 超声辅助离子液体分散液相微萃取-高效液相色谱法测定废水中雌激素的研究[J]. 分析测试技术与仪器,2009,15(3):151-157.

[10] WANG Ying,XIAO Yao,REN Ruibing,et al. Homogeneous Ionic Liquid Microextraction of Fleroxacin and Sulfaquinoxaline from Water Samples[J]. Chem J Chinese Univ,2010,9(31):1721-1724(in Chinese).

王影，肖瑶，任瑞冰,等. 水样中氟罗沙星和磺胺喹噁啉的离子液体均匀提取[J]. 高等学校化学学报,2010,9(31):1721-1724.

[11] Chun S,Dzyuba S V,Bartsch R A. Influence of Structural Variation in Room-Temperature Ionic Liquids on the Selectivity and Efficiency of Competitive Alkali Metal Salt Extraction by a Crown Ether[J]. Anal Chem,2001,73:3737-3741.

[12] DU Liming,JIN Weijun,DONG Chuan,et al. Studies on Correlation Between Protonation and Tautomerism and Luminescence Characteristics of Quinolone[J]. Spectrosc Spectr Anal,2001,21(4):518-520(in Chinese).

杜黎明,晋卫军,董川，等. 喹诺酮类药物的质子化作用及互变异构现象与荧光特性的相关性研究[J]. 光谱学与光谱分析，2001,21(4):518-520

[13] Visser A E,Swatloski R P,Reichert W M,et al. Traditional Extractions in Notraditional Solvents:Groups 1 and 2 Extraction by Crown Ethers in Room-temperature Ionic Liquids[J]. Ind Eng Chem Res,2000,39:3596-3604.

[1]	李慧慧, 姚开胜, 赵亚南, 范李娜, 田钰琳, 卢伟伟. 离子液体调控合成Pt-Pd双金属纳米材料及其催化氨硼烷水解释氢[J]. 应用化学, 2023, 40(4): 597-609.
[2]	陈启航, 许飞健, 王锋, 傅双婵, 于英豪. 低共熔溶剂及其在抗静电领域中应用的研究进展[J]. 应用化学, 2023, 40(3): 341-359.
[3]	吴双, 赵德扬, 吴胜寒, 魏立纲, 刘娜, 安庆大. 1-丁基-3-甲基咪唑甲基磺酸盐水溶液中酚型木质素单体溶解的二维相关红外光谱分析[J]. 应用化学, 2022, 39(10): 1600-1609.
[4]	何欧文, 孙长富, 于宏兵. 廉价离子液体体系中玉米芯生成糠醛优化[J]. 应用化学, 2022, 39(02): 272-282.
[5]	钮占宁, 唐好庆, 郑超, 田甜, 郑立允. 密度泛函理论研究烷基乙醇仲胺溴离子液体表面改性四氧化三铁[J]. 应用化学, 2021, 38(7): 825-835.
[6]	周超, 生程钜, 闻林林. 咪唑盐类聚离子液体抗菌剂的制备及其在水凝胶敷料中的应用[J]. 应用化学, 2021, 38(1): 51-59.
[7]	刘宁, 王丹凤, 伍素云, 刘水林, 付琳, 刘跃进. 短孔道介孔分子筛Zr-Ce-SBA-15固载酸性离子液体催化合成双酚F[J]. 应用化学, 2020, 37(9): 1038-1047.
[8]	郭辉, 殷园园, 张学颖, 庄玉伟, 曹健, 张国宝. 酸性离子液体催化合成N-氰乙基-N-羟乙基苯胺[J]. 应用化学, 2020, 37(5): 512-517.
[9]	马浩, 赵雪, 李坤兰, 邵国林, 安庆大, 杨丽玉, 魏立纲. 硅烷基咪唑双三氟甲烷磺酰亚胺离子液体气相色谱固定相的性能评价[J]. 应用化学, 2020, 37(4): 447-454.
[10]	喻昌木, 张荣, 卢小鸾, 杨敏, 彭黔荣. 具有过氧化物酶活性的Imm-Fe³⁺-IL的制备及用于比色法测定H₂O₂和葡萄糖[J]. 应用化学, 2020, 37(10): 1211-1220.
[11]	高博, 杨宏伟, 田少鹏, 赵玉真, 田甜. 1-烷基-4-氨基-1,2,4-三唑类含能离子液体的溶解性能[J]. 应用化学, 2019, 36(9): 1044-1052.
[12]	宋飞跃, 薛泳波, 高欣, 白玲, 李靖, 邓芸, 谢利娟, 阮文权. 不同离子液体双水相萃取钯[J]. 应用化学, 2019, 36(3): 335-340.
[13]	郭一江, 陈庆德, 沈兴海. 新型离子液体1-烷基-3-甲基咪唑苯甲酰基三氟硼酸盐的合成与性质[J]. 应用化学, 2019, 36(10): 1186-1193.
[14]	朱云, 洪亮, 金葆康. 高温红外光谱电化学薄层池的制作与表征[J]. 应用化学, 2019, 36(1): 107-113.
[15]	屈浩楠, 暴冲, 马文静, 马一鸣, 赵鹏, 王新海, 周艳梅. 负载1-丁基-3-甲基咪唑氯的固体炭磺酸催化水解纤维素[J]. 应用化学, 2019, 36(1): 58-64.