离子色谱法测定别嘌醇中吗啉残留

Determination of morpholine residues in allopurinol by ion chromatography

目的 建立了别嘌醇中痕量吗啉测定的离子色谱方法。方法 采用IonPac CS12(250mm×4.0 mm)阳离子色谱柱;以8~40 mmol·L^(-1)甲烷磺酸溶液洗脱;流速为1.0 mL·min^(-1);进样量为500μL;柱温为30℃;抑制器为CERS 300(4 mm);抑制电流为161 mA;外标法定量。结果 该方法下,空白溶液和别嘌醇均不干扰吗啉的检测。吗啉在0.001 487~0.014 87μg·mL^(-1)与峰面积呈现良好的线性关系(r=0.9991),加样回收率(n=3)在89.99%~118.00%,定量限为1.487 ng·mL^(-1)。室温条件下,吗啉对照品溶液和加标样品溶液分别在46.5 h、38 h内稳定性良好。结论 建立的方法灵敏、准确、专属性强、耐用性好,可用于别嘌醇中痕量吗啉的检测。

Objective To establish an ion chromatographic method for the determination of morpholine residues in allopurinol.Methods IonPac CS12 column(250 mm×4.0 mm) was used,and 8 ~ 40 mmol·L^(-1) methanesulfonic acid was used as the mobile phases in gradient elution.The flow rate was 1.0 mL·min^(-1).The injection volume was 500 μL.The column temperature was 30 ℃.The analyte was detected conductively with a CERS 300(4 mm),and the current of inhibitor was 161 mA.External standard method was used to determine the content of morpholine.Results The blank solvent and allopurinol caused no interference.The calibration curve had good linearity for morpholine at 0.001 487 ~ 0.014 87 μg·mL^(-1)(r = 0.9991).The recoveries of morpholine ranged at 89.99% ~ 118.00%(n = 3),and the limit of quantitation(LOQ) was 1.487 ng·mL^(-1).The control solution and the labeled sample solution of morpholine were stable at room temperature within 46.5 h and 38 h,respectively.Conclusion The method is sensitive,and accurate with good specialization and durability,which can be used to determine morpholine residues in allopurinol.