摘要
目的:建立离子色谱-直接电导法测定坎地沙坦酯中叠氮化钠和四丁基溴化铵残留。方法:坎地沙坦酯经二氯甲烷溶解后加水进行萃取,水相经C18固相萃取小柱萃取后直接进样。采用氢氧化钾溶液为淋洗液进行梯度洗脱,以Ionpac AS18(4 mm×250 mm)色谱柱及相应的Ionpac AG18(4 mm×50 mm)保护柱进行分离,流速为1.0 mL·min^-1,ASRS 500-4 mm阴离子抑制器和电导检测器抑制并直接检测,抑制电流99 mA,柱温35℃,进样体积200μL。结果:叠氮根离子、溴离子与其他成分的分离度良好,叠氮根质量浓度在2.33~932 ng·mL^-1范围内线性关系良好(r=0.999 6),检测下限(S/N=3)为0.699 ng·mL^-1,定量下限(S/N=10)为2.33 ng·mL^-1;溴离子质量浓度在4.8~240 ng·mL^-1范围内线性关系良好(r=0.999 5),检测下限(S/N=3)为1.44 ng·mL^-1,定量下限(S/N=10)为4.8 ng·mL^-1。共进行9批样品检测,其中4批样品含有叠氮化钠或四丁基溴化铵。结论:本方法操作简单,灵敏度高,重复性好,可用于坎地沙坦酯中叠氮化钠和四丁基溴化铵残留的检测。
Objective:To establish an ion chromatography method for the determation of sodium azide and tetrabutylammonium bromide residues in candesartan cilexetil. Methods:After being dissolved by dichlomethane,being extracted by water being and filtrated by a C18 solid phase extraction column,the samples were loaded onto the instrument.The determination was performed on an Ionpac AS18(4 mm×250 mm)column with an IonpacAG18(4 mm×50 mm)guard column. Gradient elution was carrying by using potassium hydroxide solution as drenching solution was carrying,at a flow rate of 1.0 mL·min^-1. The azide ion and bromide ion were detected by suppressed conductivity with an ASRS 500-4 mm suppressor at a current of 99 mA,the column temperature was 35 ℃ and the injection volume was 200 μL. Results:The azide ion,bromide ion and other components were well separated. The azide ion calibration curves showed good linearity in the range of 2.33-932 ng·mL^-1(r=0.999 6),the limit of detection(S/N=3)was 0.699 ng·mL^-1 and the limit of quantification(S/N=10)was 2.33 ng·mL^-1. The bromide ion calibration curves showed good linearity in the range of 4.8-240 ng·mL-1(r=0.999 5),the limit of detection(S/N=3)was 1.44 ng·mL^-1 and the limit of quantification(S/N=10)was 4.8 ng·mL^-1.There was a good resolution between azide ion and bromide ion with other components. Sodium azide and tetrabutylammonium bromide residues in 4 of 9 batches samples were detected. Conclusion:The method has the advantages of simple operation,high sensitivity,good reproducibility,and can be used for the detection of sodium azide and tetrabutylammonium bromide residues in candesartan cilexetil drugs.
作者
林群峰
许洁
栾路军
LIN Qun-feng;XU Jie;LUAN Lu-jun(No.970 Hospital of Chinese People’s Liberation Army,Weihai 264205,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2019年第12期2221-2227,共7页
Chinese Journal of Pharmaceutical Analysis
