离子色谱-抑制电导\蒸发光散射法测定阿仑膦酸钠及有关物质质量浓度

采用离子色谱-蒸发光散射法,研究阿仑膦酸钠及有关物质的色谱分离与分析方法.以IonPac AG18(2mm×50mm)和AS18(2mm×250mm)阴离子交换柱为分离柱,KOH梯度淋洗,通过抑制器将KOH转化为水,然后分别采用抑制电导和蒸发光散射器检测器检测.经优化,以信噪比(S/N)为3计算检出限,电导检测F-、Cl-、SO24-、阿仑膦酸钠、蒸发光散射检测阿仑膦酸钠的检出限分别为1.372 12×10-4、6.293 7×10-4、9.041 1×10-4、1.252 5×10-2和5.007 4μg.mL-1,相关系数分别为0.999 2、0.999 1、0.999 7、0.999 9和0.998 1,加标回收率为93.0%～109.7%.用所建立的方法可用于阿仑膦酸钠及有关物质质量浓度分析,结果令人满意.

Determination of alendronate and its related substances by lon chromatography with suppressed conducitivity and evaporative light scattering detection

Determination of Alendronate and its related substances has been evaluated using ion chromatography(IC) coupled with evaporative light scattering detector(ELSD-2000) without derivatization.IonPac AG18(2 mm×50 mm)and AS18(2 mm×250 mm)were used,a KOH eluent generator was used for gradient elution and suppressed eluent into water.After investigated condition of separation and detection,an optimized method was established.And the linearity,reproducibility,and the limit of detection(LOD) for Alendronate and its related substances were further evaluated.Regression equations revealed acceptable linearity(correlation coefficients=0.9981-0.9999) across the working-standard range(50-1 000 μg·mL-1 for Alendronate) and LODs of F-、Cl-、SO2-4 with suppressed conductivity were 1.372 12×10-4 μg·mL-1,6.293 7×10-4 μg·mL-1,9.041 1×10-4 μg·mL-1,respectively,Alendronate was 1.252 5×10-2μg·mL-1(conductivity detection) and 5.007 4 μg·mL-1(evaporative light scattering detector).The recoveries were between 93.0 %~109.7 %(n=3).This method has successfully been applied to the determination of Alendronate and its related substances.