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

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200 μL。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.

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