磷酸蒸馏-离子色谱法测定药物中的氰根总量

Determination of Total Cyanide in Drugs by Ion Chromatography Combined with Phosphoric Acid Distillation

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(250mm×4mm)和IonPac AG11-HC保护柱(50mm×4mm),流量1.0mL·min^-1,4mmol·L^-1氢氧化钠淋洗液。氰根的质量浓度在0.02~1.0mg·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。

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(3 S/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.