Determination of Total Cyanide in Drugs by Ion Chromatography Combined with Phosphoric Acid Distillation
摘 要
建立了磷酸蒸馏-离子色谱法测定药物中氰根总量的方法。样品在加入磷酸的环境下,加热蒸馏,将氰根转化成氰化氢的形式被蒸馏出来,经过冷凝管后被氢氧化钠溶液吸收。吸收液用离子色谱-安培检测器测定氰根含量。离子色谱条件:IonPac AS11-HC色谱柱(250 mm×4 mm)和IonPac AG11-HC保护柱(50 mm×4 mm),流量1.0 mL·min-1,4 mmol·L-1氢氧化钠淋洗液。氰根的质量浓度在0.02~1.0 mg·L-1内与其峰面积之间呈线性关系,相关系数为0.999 7,检出限(3S/N)为0.004 mg·L-1,样品的加标回收率为100%~102%,相对标准偏差(n=6)为1.0%~2.1%。该方法灵敏度好、精密度和重复性高,有效避免了药物基体的干扰,为难以消除的基体药物中氰根的测定提供新方法和新思路。
Abstract
A method was developed for the determination of total cyanide in drugs by ion chromatography combined with phosphoric acid distillation. The samples were heated and distilled in a phosphoric acid solution, and the hydrogen cyanide evaporated was absorbed by the sodium hydroxide solution. The cyanide (CN-) in the solution was determinated by ion chromatography with amperometric detector. Ion chromatographic condition:IonPac AS11-HC chromatographic column (250 mm×4 mm) and IonPac AG11-HC protect column (50 mm×4 mm) were used with the mobile phase of 4 mmol·L-1 NaOH solution, and the flow rate was 1.0 mL·min-1. Linear relationship between values of peak area and the mass concentration of CN- was found in the range of 0.02-1.0 mg·L-1 with correlation coefficient of 0.999 7. Values of detection limit (3S/N) for CN- was 0.004 mg·L-1. The recovery of sample ranged from 100% to 102%, and the RSDs (n=6) ranged from 1.0% to 2.1%. The method is sensitive, high precision and good repeatability. The method avoids the interference of matrix in drugs to the determination of cyanide,which is successfully used for the determination of cyanide in drugs.
中图分类号 O657.7 DOI 10.11973/lhjy-hx202004007
所属栏目 工作简报
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收稿日期 2019/8/26
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备注栾绍嵘,高级工程师,博士,研究方向为色谱分析技术
引用该论文: LUAN Shaorong,LIU Pengyu,ZHANG Fangfang,SOLANGE Muhayimana,NI Lijun. Determination of Total Cyanide in Drugs by Ion Chromatography Combined with Phosphoric Acid Distillation[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(4): 415~418
栾绍嵘,刘鹏宇,张芳芳,SOLANGEMuhayimana,倪力军. 磷酸蒸馏-离子色谱法测定药物中的氰根总量[J]. 理化检验-化学分册, 2020, 56(4): 415~418
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参考文献
【1】CUMMINGS T F. The treatment of cyanide poisoning[J]. Occupational Medicine, 2004,54(2):82-85.
【2】DAI X W, SIMONS A, BREUER P. A review of copper cyanide recovery technologies for the cyanidation of copper containing gold ores[J]. Minerals Engineering, 2012,25(1):1-13.
【3】李美君,汪秀林,姚仙珍,等.离子色谱法测定厄贝沙坦中氰化物[J].中南药学, 2013,11(2):132-134.
【4】CUI J Q, WANG X J, YUAN Y L, et al. Combined ozone oxidation and biological aerated filter processes for treatment of cyanide containing electroplating wastewater[J]. Chemical Engineering Journal, 2014,241:184-189.
【5】XIE Y S, DING Y B, LI X, et al. Selective,sensitive and reversible "turn-on" fluorescent cyanide probes based on 2,2'-dipyridylaminoanthracene-Cu2+ ensembles[J]. Chemical Communications, 2012,48(94):11513-11513.
【6】GAO Y, PAN L, SUN Y, et al. Resistance to quinclorac caused by the enhanced ability to detoxify cyanide and its molecular mechanism in Echinochloa crus-galli var.zelayensis[J]. Pesticide Biochemistry and Physiology, 2017,143:231-238.
【7】TIVANA L D, FRANCISCO J D C, ZELDER F, et al. Straightforward rapid spectrophotometric quantification of total cyanogenic glycosides in fresh and processed cassava products[J]. Food Chemistry, 2014,158:20-27.
【8】CAMPANELLA B, BIANCALANA L, DULIVO L, et al. Determination of total cyanide in soil by isotope dilution GC/MS following pentafluorobenzyl derivatization[J]. Analytica Chimica Acta, 2017,961:74-81.
【9】朱友,蔚亦沛,别振英,等.金属络合衍生-高效液相色谱法测定卷烟主流烟气中的氰化氢[J].中国烟草科学, 2015,36(5):74-78.
【10】CHEN B, DING Y B, LI X, et al. Steric hindrance-enforced distortion as a general strategy for the design of fluorescence "turn-on" cyanide probes[J]. Chemical Communications, 2013,49(86):10136-10138.
【11】姜汉硕,赵婉婧,蒋莹.连续流动注射分析法测定白酒中氰化物[J].中国食品卫生杂志, 2016,28(4):476-479.
【12】KHAJEHSHARIFI H, BORDBAR M M. A highly selective chemosensor for detection and determination of cyanide by using an indicator displacement assay and PC-ANN and its logic gate behavior[J]. Sensorsand Actuators B:Chemical, 2015,209:1015-1022.
【13】李悦,李彦懿,肖得力.氰化物定量检测方法应用研究进展[J].药物分析杂志, 2016,36(12):2075-2083.
【14】倪力军,刘建云,陈筑,等.多次高温裂解、富集-离子色谱法检测己内酰胺中的痕量氯[J].色谱, 2017,35(3):314-317.
【15】倪力军,张芳芳,栾绍嵘.高温裂解-离子色谱技术的研究进展[J].色谱, 2018,36(3):209-215.
【16】甘子琼,刘军军,唐胜利.离子色谱法同时测定火场爆炸残留物中9种典型阴离子[J].色谱, 2018,36(3):299-302.
【17】龙素群,钟志京,刘秀华,等.离子色谱法测定氰化物方法研究[J].四川大学学报(自然科学版), 2006,43(6):1352-1356.
【18】ROCKLIN R D, JOHNSON E L. Determination of cyanide, sulfide, iodide, and bromide by ion chromatography with electrochemical detection[J]. Analytical Chemistry, 1983,55(1):4-7.
【19】WU W L, XIAO Q W, ZHANG P, et al. Rapid measurement of free cyanide in liquor by ion chromatography with pulsed amperometric detection[J]. Food Chemistry, 2015,172:681-684.
【20】鲁蕴甜.离子色谱-电化学检测器测定电镀废水中的氰化物[J].广州化工, 2014,42(12):156-158.
【21】MEHER A K, LABHSETWAR N, BANSIWAL A. An improved method for direct estimation of free cyanide in drinking water by Ion Chromatography-Pulsed Amperometry Detection (IC-PAD) on gold working electrode[J]. Food Chemistry, 2018,240:131-138.
【22】CHRISTISON T T, ROHRER J S. Direct determination of free cyanide in drinking water by ion chromatography with pulsed amperometric detection[J]. Journal of Chromatography A, 2007,1155(1):31-39.
【23】林冬,郭晶晶,王鑫.安培检测-离子色谱法测定固废中痕量氰根离子[J].广州化工, 2017,45(18):95-97.
【2】DAI X W, SIMONS A, BREUER P. A review of copper cyanide recovery technologies for the cyanidation of copper containing gold ores[J]. Minerals Engineering, 2012,25(1):1-13.
【3】李美君,汪秀林,姚仙珍,等.离子色谱法测定厄贝沙坦中氰化物[J].中南药学, 2013,11(2):132-134.
【4】CUI J Q, WANG X J, YUAN Y L, et al. Combined ozone oxidation and biological aerated filter processes for treatment of cyanide containing electroplating wastewater[J]. Chemical Engineering Journal, 2014,241:184-189.
【5】XIE Y S, DING Y B, LI X, et al. Selective,sensitive and reversible "turn-on" fluorescent cyanide probes based on 2,2'-dipyridylaminoanthracene-Cu2+ ensembles[J]. Chemical Communications, 2012,48(94):11513-11513.
【6】GAO Y, PAN L, SUN Y, et al. Resistance to quinclorac caused by the enhanced ability to detoxify cyanide and its molecular mechanism in Echinochloa crus-galli var.zelayensis[J]. Pesticide Biochemistry and Physiology, 2017,143:231-238.
【7】TIVANA L D, FRANCISCO J D C, ZELDER F, et al. Straightforward rapid spectrophotometric quantification of total cyanogenic glycosides in fresh and processed cassava products[J]. Food Chemistry, 2014,158:20-27.
【8】CAMPANELLA B, BIANCALANA L, DULIVO L, et al. Determination of total cyanide in soil by isotope dilution GC/MS following pentafluorobenzyl derivatization[J]. Analytica Chimica Acta, 2017,961:74-81.
【9】朱友,蔚亦沛,别振英,等.金属络合衍生-高效液相色谱法测定卷烟主流烟气中的氰化氢[J].中国烟草科学, 2015,36(5):74-78.
【10】CHEN B, DING Y B, LI X, et al. Steric hindrance-enforced distortion as a general strategy for the design of fluorescence "turn-on" cyanide probes[J]. Chemical Communications, 2013,49(86):10136-10138.
【11】姜汉硕,赵婉婧,蒋莹.连续流动注射分析法测定白酒中氰化物[J].中国食品卫生杂志, 2016,28(4):476-479.
【12】KHAJEHSHARIFI H, BORDBAR M M. A highly selective chemosensor for detection and determination of cyanide by using an indicator displacement assay and PC-ANN and its logic gate behavior[J]. Sensorsand Actuators B:Chemical, 2015,209:1015-1022.
【13】李悦,李彦懿,肖得力.氰化物定量检测方法应用研究进展[J].药物分析杂志, 2016,36(12):2075-2083.
【14】倪力军,刘建云,陈筑,等.多次高温裂解、富集-离子色谱法检测己内酰胺中的痕量氯[J].色谱, 2017,35(3):314-317.
【15】倪力军,张芳芳,栾绍嵘.高温裂解-离子色谱技术的研究进展[J].色谱, 2018,36(3):209-215.
【16】甘子琼,刘军军,唐胜利.离子色谱法同时测定火场爆炸残留物中9种典型阴离子[J].色谱, 2018,36(3):299-302.
【17】龙素群,钟志京,刘秀华,等.离子色谱法测定氰化物方法研究[J].四川大学学报(自然科学版), 2006,43(6):1352-1356.
【18】ROCKLIN R D, JOHNSON E L. Determination of cyanide, sulfide, iodide, and bromide by ion chromatography with electrochemical detection[J]. Analytical Chemistry, 1983,55(1):4-7.
【19】WU W L, XIAO Q W, ZHANG P, et al. Rapid measurement of free cyanide in liquor by ion chromatography with pulsed amperometric detection[J]. Food Chemistry, 2015,172:681-684.
【20】鲁蕴甜.离子色谱-电化学检测器测定电镀废水中的氰化物[J].广州化工, 2014,42(12):156-158.
【21】MEHER A K, LABHSETWAR N, BANSIWAL A. An improved method for direct estimation of free cyanide in drinking water by Ion Chromatography-Pulsed Amperometry Detection (IC-PAD) on gold working electrode[J]. Food Chemistry, 2018,240:131-138.
【22】CHRISTISON T T, ROHRER J S. Direct determination of free cyanide in drinking water by ion chromatography with pulsed amperometric detection[J]. Journal of Chromatography A, 2007,1155(1):31-39.
【23】林冬,郭晶晶,王鑫.安培检测-离子色谱法测定固废中痕量氰根离子[J].广州化工, 2017,45(18):95-97.
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