乙醇-正丙醇-磷酸二氢钠多元混合双水相体系萃取/检测湖水中的诺氟沙星残留

doi:10.19894/j.issn.1000-0518.200331

摘要/Abstract

摘要： 构建了乙醇-正丙醇-磷酸二氢钠(NaH₂PO₄)多元混合双水相体系萃取/检测环境水样中的诺氟沙星,讨论了醇的用量、盐的种类及浓度、pH值、温度对诺氟沙星分配行为的影响,并采用响应曲面法(Response surface methodology,RSM)对实验条件进行优化。结果表明,在乙醇与正丙醇加入量为4 mL(体积比为1∶1),NaH₂PO₄的浓度为0.200 g/mL,温度为30 ℃,pH=5的最优条件下,诺氟沙星的萃取率为94.34 %。该多元双水相体系较单元双水相体系相比,目标物的萃取率明显提升。

关键词: 多元混合双水相, 小分子醇, 萃取/检测, 诺氟沙星

Abstract: A binary aqueous two-phase system (ATPS) based on ethanol-1-propanol-NaH₂PO₄ system was constructed and applied for the separation and determination of norfloxacin (NOR) in real water samples. The influence factors on partition behaviors of NOR were discussed, including the types and the concentration of phase salts, the volume ratio of alcohols, the pH value and extraction temperature. The response surface methodology was used to determine the best experimental conditions for multi-factor experiments. The study shows that when the concentration of NaH₂PO₄ is 0.200 g/mL, the volume of ethanol is 2 mL (the volume ratio of alcohols is 1∶1) , pH value is 5, and the extraction temperature is 30 ℃, the extraction efficiency of NOR reaches 94.34%. Compared with the unit aqueous two-phase system, the extraction efficiency of the target compound by the multi-component aqueous two-phase system constructed in this paper is obviously improved.

Key words: Multi-component mixed aqueous two-phase system, Small molecule alcohol, Extraction/detection, Norfloxacin

中图分类号:

O658.2

郭东刚, 倪良, 王良. 乙醇-正丙醇-磷酸二氢钠多元混合双水相体系萃取/检测湖水中的诺氟沙星残留[J]. 应用化学, 2021, 38(7): 847-856.

GUO Dong-Gang, NI Liang, WANG Liang. Separation and Determination of Norfloxacin in Real Water Samples Using Binary Small Molecule Alcohol-Salt Aqueous Two-Phase System Coupled with High Performance Liquid Chromatography[J]. Chinese Journal of Applied Chemistry, 2021, 38(7): 847-856.

参考文献

[1] 李俊, 杨玉琴, 王英瑛. 中国药典2015年版中诺氟沙星胶囊有关物质测定方法的改进研究[J]. 中国现代应用药学, 2019, 36(6): 714-717.
LI J, YANG Y Q, WANG Y Y. Improvement of the determination method of related substances of norfloxacin capsules in chinese pharmacopoeia (2015 Edition) [J]. Chinese J Mod Appl Pharm, 2019, 36(6): 714-717.
[2] 陈卫平, 彭程伟, 杨阳, 等. 北京市地下水中典型抗生素分布特征与潜在风险[J]. 环境科学, 2017, 38(12): 5074-5080.
CHEN W P, PENG C W, YANG Y, et al. Distribution characteristics and risk analysis of antibiotic in the groundwater in Beijing [J]. Environ Chem, 2017, 38(12): 5074-5080.
[3] 王良, 荆雨众. 双水相萃取抗生素的应用研究进展[J]. 现代化工, 2016,2:34-36, 38.
WANG L, JING Y Z. Research progress of aqueous two-phase extraction of antibiotics[J]. Mod Chem Ind, 2016, 2: 34-36, 38.
[4] 冯志彪, 屈玉霄, 张晓庆, 等. 亲水有机溶剂-盐双水相体系分离乳清蛋白抗氧化性多肽[J]. 中国食品学报, 2018, 18(10): 170-177.
FENG Z B, QU Y X, ZHANG X Q, et al. Separation of antioxidant peptides in pepsin-catalyzed hydrolysis of whey protein isolate using aqueous two-phase systems [J]. J Chinese Inst Food Sci Tech, 2018, 18(10): 170-177.
[5] LI Z G, TENG H, XIU Z L. Extraction of 1,3-propanediol from glycerol-based fermentation broths with methanol/phosphate aqueous two-phase system[J]. Process Biochem, 2011, 46(2): 586-591.
[6] AZEVEDO A M, ROSA P A J, FERRIRA I F, et al. Chromatography-free recovery of biopharmaceuticals through aqueous two-phase processing[J]. Trends Biotechnol, 2009, 27(4): 240-247.
[7] BULGARIU L, BULGARIU D. Extraction of gold(III) from chloride media in aqueous polyethylene glycol-based two-phase system[J]. Sep Purif Technol, 2011, 80(3): 620-625.
[8] SALABAT A, SADEGHI R, MOGHADAM S T, et al. Partitioning of L-methionine in aqueous two-phase systems containing poly(propylene glycol) and sodium phosphate salts[J]. J Chem Thermodyn, 2011, 43(10): 1525-1529.
[9] 赵晓军, 王钰伟, 武大引. 双水相气浮溶剂浮选-紫外分光光度法测定水中痕量氯霉素[J]. 应用化工, 2015, ^: 1358-1362.
ZHAO X J ,WANG Y W,WU D Y. UV-Vis spectrophotometric determination trace chloramphenicol in water by aqueous two-phase gas solvent sublation[J]. Appl Chem Ind, 2015, 44(7): 1358-1362.
[10] LU Y M, LU W J, WANG W, et al. Thermodynamic studies of partitioning behavior of cytochrome in ionic liquid-based aqueous two-phase system[J]. Talanta, 2011, 85(3): 1621-1626.
[11] LSARAVANAN S, RAO J R, NAIR B U, et al. Aqueous two-phase poly(ethylene glycol)-poly(acrylic acid) system for protein partitioning: influence of molecular weight, pH and temperature[J]. Process Biochem, 2008, 43 (9): 905-911.
[12] LU Y, HAN J, TAN Z J, et al. Measurement and correlation of phase equilibria in aqueous two-phase systems containing polyoxyethylene lauryl ether and three kinds of potassium salts at different temperatures[J]. J Chem Eng Data, 2013, 58(1): 118-127.
[13] PIRDASHTI M, MOVAGHARNEJAD K, ROSTAMI A A, et al. Liquid-liquid equilibria, electrical conductivity, and refractive indices of poly(ethylene glycol)+sodium sulfate+guanidine hydrochloride aqueous two-phase systems: correlation and thermodynamic modeling[J]. Fluid Phase Equilib, 2016, 417: 29-40.
[14] 姚以亮. 离子液体/聚合物/小分子有机溶剂双水相体系的构建及其分离富集抗生素的机理研究[D]. 西安: 长安大学, 2016.
YAO Y L. Construction of aqueous two-phase systems base on ionic liquids/ polymers/ small molecule organic solvents for the separation and concentration of antibiotics[D]. Xi′an: Chang′an University, 2016.
[15] DUPONT J, CONSORTI C S, SUAREZ P A Z, et al. Preparation of 1-butyl-3-methyl imidazolium-based room temperature ionic liquids[J]. Org Synth, 2002, 79: 236-241.
[16] 关卫省, 邓江华, 韩娟. (乙醇+丙酮)-硫酸铵二元双水相分离萃取盐酸四环素[J]. 环境化学, 2013, 32(3): 513-517.
GUAN W S, DENG J H, HAN J. Ethanol and acetone-ammonium sulfate binary aqueous two-phase extraction separation of tetracycline[J]. Environ Chem, 2013, 32(3): 513-517.
[17] 关卫省, 邓江华, 韩娟. 醇和小分子有机物二元双水相体系萃取盐酸多西环素[J]. 应用化工, 2012, 41(6): 992-995, 999.
GUAN W S, DENG J H, HAN J. Extraction of doxycycline hydrochloride using anhydrous alcohol and acetone binary aqueous two phase system[J]. Appl Chem Ind, 2012, 41(6): 992-995, 999.
[18] WU X Y, LIU Y, ZHAO Y J. Effect of salt type and alkyl chain length on the binodal curve of an aqueous two-phase system composed of imidazolium ionic liquids[J]. J Chem Eng Data, 2018, 63 (9): 3297-3304.
[19] MOHAMMED T Z M, SHOLEH H. Salting-out effect, preferential exclusion, and phase separation in aqueous solutions of Chaotropic water-miscible ionic liquids and Kosmotropic salts: effects of temperature, anions, and cations[J]. J Chem Eng Data, 2010, 55(4): 1598-1610.
[20] 郭东刚, 邵丽, 杨旭, 等. 小分子有机溶剂双水相在分离分析中应用研究进展[J]. 化学世界, 2016, 57(5): 313-316, 320.
GUO D G, SHAO L, YANG X, et al. Research progress of application of small molecule organic solvent in separation and analysis[J]. Chem World, 2016, 57(5): 313-316,320.
[21] FERREIRA M C, BESSA L C B A, MEIRELLES A J A, et al. Liquid-liquid equilibrium during ethanolysis of soybean oil[J]. Fluid Phase Equilibria, 2018, 473(2): 286-293.