HPLC法测定泊沙康唑注射液中乙二胺四乙酸二钠的含量
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摘要
建立了高效液相色谱法测定泊沙康唑注射液中的螯合剂乙二胺四乙酸二钠(EDTA-2Na)。供试品溶液加铜离子(Cu~(2+))络合EDTA-2Na、加碱超声沉淀泊沙康唑。采用Eclipse XDB C_(18)色谱柱,流动相为乙腈:20 mmol/L四丁基硫酸氢铵(TBAHS,用氢氧化钠调至pH 3.0):水,梯度洗脱,柱温30℃,紫外检测波长254nm,流速0.8 ml/min,进样量5μl。EDTA-2Na在0.5～30μg/ml浓度范围内线性关系良好(r~2=0.999 5)。平均回收率为100.0%,RSD为0.91%。
An HPLC method was established for the determination of disodium edetate(EDTA-2 Na)in posaconazole injection.Sample solution was treated by chelation with Cu~(2+),precipitation with sodium hydroxide solution under ultrosonic.An Eclipse XDB C,8 column was used,with the mobile phase of acetonitrile:20 mmol/L tetrabutylammonium hydrogen sulfate(TBAHS,adjusted to pH 3.0 with sodium hydroxide):water using gradient elution.The column temperature was 30℃,the detection wavelength was 254 nm and the flow rate was 0.8 ml/min,the amount of injection was 5μl.It was linear for EDTA-2 Na in the range of 0.5-30μg/ml.The average recovery was 100.0%,with RSD of 0.91%.
An HPLC method was established for the determination of disodium edetate(EDTA-2 Na)in posaconazole injection.Sample solution was treated by chelation with Cu~(2+),precipitation with sodium hydroxide solution under ultrosonic.An Eclipse XDB C,8 column was used,with the mobile phase of acetonitrile:20 mmol/L tetrabutylammonium hydrogen sulfate(TBAHS,adjusted to pH 3.0 with sodium hydroxide):water using gradient elution.The column temperature was 30℃,the detection wavelength was 254 nm and the flow rate was 0.8 ml/min,the amount of injection was 5μl.It was linear for EDTA-2 Na in the range of 0.5-30μg/ml.The average recovery was 100.0%,with RSD of 0.91%.
引文
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[11]CALTABIANO A M.Quantitation of sulfobutyl ether-pcyclodextrin(Captisol~(TM))in Vestipitant IV solution by liquid chromatography with ultraviolet(UV)detection[J].J Pharm Biomed Anal,2016,118(25):276-283.
[2]刁岩忠,韩继永,陈祥峰.HPLC法测定注射用泮托拉唑钠中乙二胺四乙酸二钠的含量[J].药物分析杂志,2011,31(2):282-284.
[3]孙春霞,韩文芳,李津.HPLC测定氯化钠滴眼液中乙二胺四乙酸二钠的含量[J].食品与药品,2015,17(4):270-272.
[4]RALPH F,TORSTEN D,BERNHARD O.Determination of EDTA in dried blood samples by tandem mass spectrometry avoids serious errors in newborn screening[J].Eur J Pediatr,2009,168(5):553-558.
[5]陈柳生,蔡自由,周伟明.离子色谱法测定维生素B_1注射液中的EDTA及硝酸根离子[J].中国实验方剂学杂志,2014,20(14):61-64.
[6]魏冬旭,胡珅,孙莹,等.高效液相色谱法测定食品中乙二胺四乙酸二钠[J].检验检疫学刊,2013,23(6):50-53.
[7]王刚,刘建平,沈艳丽.HPLC-ELSD法测定注射用福沙匹坦二甲葡胺中聚山梨酯80和EDTA的含量[J].药学研究,2016,35(3):151-153.
[8]NGIM K K,GU Z,CATALANO T.Characterization and resolution of reversed phase HPLC chromatography failure attributed to sulfobutylether-beta-cyclodextrin in a pharmaceutical sample preparation[J].J Pharm Biomed Anal,2009,49(3):660-669.
[9]LEONG N J,PRANKERD R J,SHACKLEFORD D M,et al.Evaluation of the impact of sulfobutylether7-β-cyclodextrin on the liquid chromatography-mass spectrometry analysis of biological samples arising from in vivo pharmacokinetic studies[J].J Pharm Sci, 2015,104(4):1561-1562.
[10]GAGE R,VENN R F,BAYLISS M A J,et al.Fluorescence determination of sulphobutylether-β-cyclodextrin in human plasma by size exclusion chromatography with inclusion complex formation[J].J Pharm Biomed Anal,2000,22(5):773-780.
[11]CALTABIANO A M.Quantitation of sulfobutyl ether-pcyclodextrin(Captisol~(TM))in Vestipitant IV solution by liquid chromatography with ultraviolet(UV)detection[J].J Pharm Biomed Anal,2016,118(25):276-283.