HPLC-ELSD和IC-ICD检测磺丁基-β-环糊精中的杂质离子

Determination of Impurity Ions in Sulfobutyl-β-cyclodextrin by HPLC-ELSD and IC-ICD

关键词:  高效液相色谱法  离子色谱  磺丁基-β-环糊精  氯化钠  4-羟基-1-丁烷磺酸钠  双(4-磺丁基)醚二钠

Key words:  HPLC  ion chromatography  sulfonbutyl-β-cyclodextrin  sodium chloride  4-hydroxy-1-butanesulfonate  bis-(4-sulfobutyl) ether disodium

摘要:

目的 建立了高效液相色谱-蒸发光散射法（HPLC-ELSD）及离子色谱-抑制电导检测法（IC-ICD）测定磺丁基-β-环糊精中氯化钠、4-羟基-1-丁烷磺酸钠、双（4-磺丁基）醚二钠3种杂质含量的方法。方法 HPLC-ELSD采用CD-Screen-IEC柱（4 mm×150 mm，3 μm），梯度洗脱，流速为1.2 mL·min^-1；IC-ICD采用Dionex IonPac AS19（4 mm×250 mm）阴离子交换色谱柱分离，30 mmol·L^-1氢氧化钠溶液为淋洗液，等度洗脱，流速为1.0 mL·min^-1。结果 2种方法各组分分离度良好，HPLC-ELSD法中氯化钠、4-羟基-1-丁烷磺酸钠、双（4-磺丁基）醚二钠检出限（S/N=3）分别为0.230，0.270和0.340 ng，IC-ICD法检出限分别为0.041，0.027和0.014 ng。结论 HPLC-ELSD和IC-ICD在磺丁基-β-环糊精中氯化钠、4-羟基-1-丁烷磺酸钠、双（4-磺丁基）醚二钠3种杂质的含量测定结果上没有明显不同，可根据实际情况选择，只是根据2种方法的检出限及定量限值，IC-ICD法灵敏度更高。

Abstract:

OBJECTIVE To establish high performance liquid chromatography-evaporative light scattering(HPLC-ELSD) and ion chromatography-inhibition conductivity detection(IC-ICD) analytical method for sodium chloride, 4-hydroxy-1-butanesulfonate and bis-(4-sulfbutyl) ether disodium of sulfonbutyl-β-cyclodextrin. METHODS HPLC-ELSD method was used for assay and related subsatances test:CD-Screen-IEC column(4 mm×150 mm, 3 μm); gradient elution; flow rate:1.2 mL·min^-1. IC-ICD method was used for assay and related subsatances test:Dionex Ionpac AS19 column(4 mm×250 mm); mobile phase:30 mmol·L^-1 sodium hydroxide solution for elution; flow rate:1.0 mL·min^-1. RESULTS Two methods had good separation of components. The S/N of sodium chloride, sodium 4-hydroxy-1-butane sulfonate and bis-(4-sulfobutyl) ether disodium in HPLC-ELSD method is 0.230, 0.270 and 0.340 ng, respectively. The limit of detection of IC-ICD is 0.041, 0.027 and 0.014 ng. CONCLUSION There is no obvious difference between HPLC-ELSD and IC-ICD in three impurities content determination of sodium chloride, 4-hydroxy-1-butanesulfonate and bis-(4-sulfobutyl) ether disodium of sulfonbutyl-β-cyclodextrin. It can be selected according to the actual situation. Only according to the detection limit and quantitative limit of the two methods, IC-ICD has higher sensitivity.