建立了离子色谱-电化学法测定坎地沙坦酯药物中羟胺残留的方法.坎地沙坦酯药物经二氯甲烷溶解后加30mmol/L甲磺酸溶液进行萃取,水相过OnGuard II RP柱后直接进样.采用30 mmol/L甲磺酸溶液为淋洗液,以lonPaCCS16(250mmx5mm)色谱柱进行分离,流速为1.0 mL/min;柱后加300mmol/L氢氧化钠溶液,流速为0.3mL/min.采用电化学检测器进行检测,电极材料为金电极,参比电极为PH-Ag/AgCl复合电极,电位波形为氨基酸六电位,柱温40℃,进样体积25μL.实验结果表明,羟胺与铵离子的分离度良好,羟胺在0.01447～0.2894mg/L范围内线性关系良好(r=0.999),检出限(LOD)为0.00724 mg/L,定量下限(LOQ)为0.014 47 mg/L.该方法操作简单、灵敏度高、重现性好,可用于坎地沙坦酯药物中羟胺残留的检测.%A method was developed for the determination of hydroxylamine residues in candesartan cilexetil drugs by ion chromatography with electrochemical detection. After dissolved with dichlometh-ane, extracted with 30 mmol/L methanesulfonic acid solution and filtrated on an OnGuard Ⅱ RP column,the samples were injected into the instrument. The separation was performed on an Ionpac CS16(250 mm x5 mm) column using 30 mmol/L methanesulfonic acid as eluting solution at a flow rate of 1.0 miymin. Then, a 300 mmol/L sodium hydroxide solution was added into the instrument at a flow rate of 0.3 mL/min. An integrated pulsed electrochemical detector was used for the detection, in which the electrode material is made of gold, the reference electrode is pH-Ag/AgCl composite electrode, the potential waveform is composed of six potentials of amino acid, the column temperature is 40 °C, and the injection volume is 25 μL. The calibration curve for hydroxylamine showed a good linearity (r =0.999) in the range of 0.014 47-0.289 4 mg/L, with a limit of detection (LOD, S/N=3) of 0.007 24 mg/L and a limit of quantitation(LOQ, S/N =10) of 0.014 47 mg/L. There was a good resolution between hydroxylamine and ammonium ion. With the advantages of simple operation, high sensitivity and good reproducibility, the method could be used for the detection of hydroxylamine residues in candesartan cilexetil drugs.
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