自制的苄氧基葫芦脲[6]应用于荧光光度法测定商业制剂中头孢曲松钠的含量
Application of Self-Prepared Benzyloxy Cucurbit[6]uril to Fluorescence Spectrophotometric Determination of Ceftriaxone Sodium in Its Commercial Preparations
摘 要
制备了苄氧基葫芦脲[6]（[BnO]2CB6），并应用于商业制剂中头孢曲松钠（CTRX）的荧光光度法测定。在pH 6.5的Britton-Robinson缓冲溶液中，[BnO]2CB6与CTRX形成包结物（包结比为1∶1），使体系发生光诱导的电子转移作用，导致明显的荧光猝灭现象。荧光反应的激发波长和发射波长依次为405，495 nm。CTRX的浓度在40 μmol·L-1以内与其对应的荧光猝灭程度呈线性关系，检出限（3S/N）为17 nmol·L-1。方法用于CTRX商业制剂样品的分析，CTRX的测定值与高效液相色谱法（HPLC）测得的结果相符，加标回收率为98.0%~101%，测定值的相对标准偏差（n=6）为3.0%~7.2%。
荧光光度法
头孢曲松钠
benzyloxy cucurbit[6]uril
fluorescence spectrophotometry
ceftriaxone sodium
Abstract
Benzyloxy cucurbit[6]uril ([BnO]2CB6) was prepared and applied to fluorescence spectrophotometric determination of ceftriaxone sodium (CTRX) in its commercial preparations. In a B-R buffer solution of pH 6.5,[BnO]2CB6 reacted with CTRX to form an inclusion complex (with mole ratio of 1 to 1), leading to photo-induced electron transfer in the system, and to obvious quenching of fluorescence. And it was found that when excited at 405 nm,fluorescence was emitted at 495 nm. Linear relationship was kept between magnitude of quenching of fluorescence intensity (ΔF) and concentration of CTRX in the range within 40 μmol·L-1, with value of detection limit (3S/N) of 17 nmol·L-1. Contents of CTRX in the samples of commercial preparations were determined by the proposed method, giving results in consistency with those given by HPLC and values of recovery found by standard addition were ranged between 98.0% and 101%, with values of RSD's (n=6) in the range of 3.0%-7.2%.
中图分类号 O657.31 DOI 10.11973/lhjy-hx201805002
所属栏目 试验与研究
基金项目 国家自然科学基金（21605001）；巢湖学院自然科学基金（XLY-201608）
收稿日期 2017/10/4
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备注王冬梅,硕士,实验师,研究方向为光电分析,laoshu029228@sohu.com
引用该论文: WANG Dongmei,SUN Junyong. Application of Self-Prepared Benzyloxy Cucurbit[6]uril to Fluorescence Spectrophotometric Determination of Ceftriaxone Sodium in Its Commercial Preparations[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(5): 502～507
王冬梅,孙军勇. 自制的苄氧基葫芦脲[6]应用于荧光光度法测定商业制剂中头孢曲松钠的含量[J]. 理化检验－化学分册, 2018, 54(5): 502～507
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参考文献
【1】ZHAO W, ZHANG Y, LI Q. Indirect spectrophotometric determination of sodium ceftriaxone with n-propyl alcohol-ammonium sulfate-water system by extraction flotation of copper(Ⅱ)[J]. Clinica Chimica Acta, 2008,391(1/2):80-84.
【2】SUN H, WANG H, GE X. Simultaneous determination of the combined drugs of Ceftriaxone sodium, Metronidazole, and Levofloxacin in human urine by high-performance liquid chromatography[J]. Journal of Clinical Laboratory Analysis, 2012,26(6):486-492.
【3】ABDEL-HAMID M E. FSQ spectrophotometric and HPLC analysis of some cephalosporins in the presence of their alkali-induced degradation products[J]. IL Farmaco, 1998,53(2):132-138.
【4】PAJCHEL G, TYSKI S. Adaptation of capillary electrophoresis to the determination of selected cephalosporins for injection[J]. Journal of Chromatography A, 2000,895(1/2):27-31.
【5】BROUWERS A, SCHIETTEKATTE G, MARIEN G, et al. Interference of ceftriaxone on capillary zone electrophoresis[J]. Clinica Chimica Acta, 2007,376(1/2):255-256.
【6】HE Y H, LV J R, ZHU X H, et al. Chemiluminescence reaction with soluble manganese(Ⅳ) as the oxidant[J]. Acta Chimica Sinica, 2005,63(8):729-733.
【7】范秉琳,倪天军,袁建梅,等.头孢曲松钠与1,2-萘醌-4-磺酸钠的光度分析及应用[J].分析科学学报, 2014,30(1):91-94.
【8】LU H, MEI L, ZHANG G, et al. Interaction between cucurbit
【9】uril and bispyridinecarboxamide[J]. Journal of Inclusion Phenomena and Macrocyclic Chemistry, 2007,59(1/2):81-90.
【10】FREEMAN W A, MOCK W L, SHIH N Y. Cucurbituril[J]. Journal of the American Chemical Society, 1981,103(24):7367-7368.
【11】MASSON E, LING X, JOSEPH R, et al. Cucurbituril chemistry:A tale of supramolecular success[J]. RSC Advances, 2012,2(4):1213-1247.
【12】MARQUEZ C, NAU W M. Two mechanisms of slow host-guest complexation between cucurbit
【13】uril and cyclohexylmethylamine:pH-Responsive supramolecular kinetics[J]. Angewandte Chemie International Edition, 2001,40(17):3155-3160.
【14】ZHAO W X, WANG C Z, ZHANG Y Q, et al. Coordination and recognition of lanthanide cations by a methyl-substituted cucurbit
【15】uril derived from 3α-methyl-glycoluril[J]. Supramolecular Chemistry, 2015,27(10):661-668.
【16】GAMAL-ELDIN M A, MACARTNEY D H. Selective molecular recognition of methylated lysines and arginines by cucurbit
【17】uril and cucurbit
【18】uril in aqueous solution[J]. Organic & Biomolecular Chemistry, 2013,11(3):488-495.
【19】GURBUZ S, IDRIS M, TUNCEL D. Cucurbituril-based supramolecular engineered nanostructured materials[J]. Organic & Biomolecular Chemistry, 2015,13(2):330-347.
【20】KARCHER S, KORNMVLLER A, JEKEL M. Cucurbituril for water treatment. Part I:Solubility of cucurbituril and sorption of reactive dyes[J]. Water Research, 2001,35(14):3309-3316.
【21】GOEHRY C, BESORA M, MASERAS F. Computational study on the mechanism of the acceleration of 1,3-dipolar cycloaddition inside cucurbit
【22】uril[J]. ACS Catalysis, 2015,5(4):2445-2451.
【23】李涛,胡青大,唐冬宝,等.苄氧基葫芦
【24】脲的合成及其结构表征[J].河北师范大学学报(自然科学版), 2015,39:419-422.
【25】JON S Y, SELVAPALAM N, OH D H, et al. Facile synthesis of cucurbit[n]uril derivatives via direct functionalization:Expanding utilization of cucurbit[n]uril[J]. Journal of the American Chemical Society, 2003,125(34):10186-10187.
【26】CONNORS K A. Binding constants:The measurement of molecular complex stability[M]. New York:John Wiley & Sons, 1987.
【27】DING X P, TANG D B, LI T, et al. A novel spectrofluorometric method for the determination of methiocarb using an amphiphilic p-sulfonatocalix
【28】arene[J]. Spectrochimica Acta Part A, 2011,81(1):44-47.
【29】ZHOU Y, XU H, YU H, et al. Spectrofluorometric study on the inclusion behavior of p-(p-carboxyl benzeneazo) calix
【30】arene with norfloxacin[J]. Spectrochimica Acta Part A, 2008,70(2):411-415.
【31】韩宝航,刘育.葫芦脲:分子识别与组装[J].有机化学, 2003,23(2):139-142.
【2】SUN H, WANG H, GE X. Simultaneous determination of the combined drugs of Ceftriaxone sodium, Metronidazole, and Levofloxacin in human urine by high-performance liquid chromatography[J]. Journal of Clinical Laboratory Analysis, 2012,26(6):486-492.
【3】ABDEL-HAMID M E. FSQ spectrophotometric and HPLC analysis of some cephalosporins in the presence of their alkali-induced degradation products[J]. IL Farmaco, 1998,53(2):132-138.
【4】PAJCHEL G, TYSKI S. Adaptation of capillary electrophoresis to the determination of selected cephalosporins for injection[J]. Journal of Chromatography A, 2000,895(1/2):27-31.
【5】BROUWERS A, SCHIETTEKATTE G, MARIEN G, et al. Interference of ceftriaxone on capillary zone electrophoresis[J]. Clinica Chimica Acta, 2007,376(1/2):255-256.
【6】HE Y H, LV J R, ZHU X H, et al. Chemiluminescence reaction with soluble manganese(Ⅳ) as the oxidant[J]. Acta Chimica Sinica, 2005,63(8):729-733.
【7】范秉琳,倪天军,袁建梅,等.头孢曲松钠与1,2-萘醌-4-磺酸钠的光度分析及应用[J].分析科学学报, 2014,30(1):91-94.
【8】LU H, MEI L, ZHANG G, et al. Interaction between cucurbit
【9】uril and bispyridinecarboxamide[J]. Journal of Inclusion Phenomena and Macrocyclic Chemistry, 2007,59(1/2):81-90.
【10】FREEMAN W A, MOCK W L, SHIH N Y. Cucurbituril[J]. Journal of the American Chemical Society, 1981,103(24):7367-7368.
【11】MASSON E, LING X, JOSEPH R, et al. Cucurbituril chemistry:A tale of supramolecular success[J]. RSC Advances, 2012,2(4):1213-1247.
【12】MARQUEZ C, NAU W M. Two mechanisms of slow host-guest complexation between cucurbit
【13】uril and cyclohexylmethylamine:pH-Responsive supramolecular kinetics[J]. Angewandte Chemie International Edition, 2001,40(17):3155-3160.
【14】ZHAO W X, WANG C Z, ZHANG Y Q, et al. Coordination and recognition of lanthanide cations by a methyl-substituted cucurbit
【15】uril derived from 3α-methyl-glycoluril[J]. Supramolecular Chemistry, 2015,27(10):661-668.
【16】GAMAL-ELDIN M A, MACARTNEY D H. Selective molecular recognition of methylated lysines and arginines by cucurbit
【17】uril and cucurbit
【18】uril in aqueous solution[J]. Organic & Biomolecular Chemistry, 2013,11(3):488-495.
【19】GURBUZ S, IDRIS M, TUNCEL D. Cucurbituril-based supramolecular engineered nanostructured materials[J]. Organic & Biomolecular Chemistry, 2015,13(2):330-347.
【20】KARCHER S, KORNMVLLER A, JEKEL M. Cucurbituril for water treatment. Part I:Solubility of cucurbituril and sorption of reactive dyes[J]. Water Research, 2001,35(14):3309-3316.
【21】GOEHRY C, BESORA M, MASERAS F. Computational study on the mechanism of the acceleration of 1,3-dipolar cycloaddition inside cucurbit
【22】uril[J]. ACS Catalysis, 2015,5(4):2445-2451.
【23】李涛,胡青大,唐冬宝,等.苄氧基葫芦
【24】脲的合成及其结构表征[J].河北师范大学学报(自然科学版), 2015,39:419-422.
【25】JON S Y, SELVAPALAM N, OH D H, et al. Facile synthesis of cucurbit[n]uril derivatives via direct functionalization:Expanding utilization of cucurbit[n]uril[J]. Journal of the American Chemical Society, 2003,125(34):10186-10187.
【26】CONNORS K A. Binding constants:The measurement of molecular complex stability[M]. New York:John Wiley & Sons, 1987.
【27】DING X P, TANG D B, LI T, et al. A novel spectrofluorometric method for the determination of methiocarb using an amphiphilic p-sulfonatocalix
【28】arene[J]. Spectrochimica Acta Part A, 2011,81(1):44-47.
【29】ZHOU Y, XU H, YU H, et al. Spectrofluorometric study on the inclusion behavior of p-(p-carboxyl benzeneazo) calix
【30】arene with norfloxacin[J]. Spectrochimica Acta Part A, 2008,70(2):411-415.
【31】韩宝航,刘育.葫芦脲:分子识别与组装[J].有机化学, 2003,23(2):139-142.
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