离子色谱安培法检测维生素B_6与2-噻吩乙酸中的氰化物

Determination of cyanide in vitamin B_6 and 2-thiopheneacetic acid drugs by ion chromatography with amperometric detector

目的:建立离子色谱积分安培法检测维生素B_6(VB_6)与2-噻吩乙酸(2-TPA)2种合成药物中的氰化物。方法:维生素B_6经甲醇溶解后,加入氢氧化钠溶液溶解萃取;2-噻吩乙酸经热氢氧化钠溶液超声溶解,定容,经0.22μm的尼龙滤膜和On Guard RP柱处理后进入离子色谱分析。使用IonPac AS18(250 mm×4 mm)阴离子交换色谱柱和IonPac AG18(50 mm×4 mm)保护柱,20 mmol·L^(-1)氢氧化钠淋洗液,安培检测器。结果:在优化的色谱条件下,水中氰在0.20~10.0 mg·L^(-1)范围内呈良好线性,线性相关系数为0.999 9,最低检出限(S/N≥3)为1.64μg·L^(-1),实际合成药物中CN-的检出限为0.016 4μg·g^(-1),样品的加标回收率为92.4%~97.9%。维生素B_6(VB_6-1,VB_6-2,VB_6-Y1,VB_6-Y2)粗产品与2-噻吩乙酸(2-TPA-1,2-TPA-2)原料样品中,VB_6-1中未检出氰化物;VB_6-2中氰离子的含量为0.823μg·g^(-1);VB_6-Y1中氰离子的含量为117.1μg·g^(-1);VB_6-Y2中氰离子的含量为1.872μg·g^(-1);2-TPA-1中氰离子的含量为118.7μg·g^(-1);2-TPA-2中未检出氰化物。因此,合成原料和粗产品中含有一定的氰化物,精制产品中的氰化物含量很低,甚至有的低于检出限而未检出。结论:本文方法前处理简单,环境友好,受其他杂质的干扰较小,灵敏度高,经方法学验证可用于评价VB_6与2-噻吩乙酸药物中氰化物的含量。

Objective： To establish a method for the determination of cyanide in vitamin B6（VB6）and 2-thiopheneacetic acid（2-TPA）drugs by ion chromatography with integrated amperometric detector.Methods： The certain quality of VB6 was dissolved in methanol and sodium hydroxide solution,2-TPA was dissolved in hot sodium hydroxide solution.All the solutions were pre-treated by 0.22 μm nylon filter membrane and a Guard RP column.The solutions were then analyzed by IC.The chromatography column was IonPac AS18（250 mm×4 mm）and IonPac AG18（50 mm×4 mm）.The eluent was 20 mmol·L-1 NaOH with 1.0 mL·min-1 flow rate.The amperometric detector was used.Results： With the optimum conditions,the CN-was linear in the range of 0.20-10.0 mg·L-1 with correlation coefficient of 0.999 9.The method LOD for CN- was 0.016 4 μg·g-1.The recoveries ranged of 92.4%-97.9%.Multiple VB6 and 2-TPA samples were assessed.The content of cyanide was not detected in VB6-1.The content of CN- was 0.823 μg·g-1 in VB6-2,117.1 μg·g-1 in VB6-Y1,1.872 μg·g-1 in VB6-Y2 and 118.7 μg·g-1 in 2-TPA-1.The content of cyanide was not detected in 2-TPA-2.Synthetic raw materials and crude products contained a certain amount of cyanide;the cyanide could not be detected or was so low in the refined products.Conclusion： By methodology verification,this method requires simple pretreatment,has high repeatability,without pollution and with little interference.This method had been applied to assess the content of cyanide in VB6 and 2-TPA.