摘要
目的:建立同时测定附子理中丸中9种无机阴离子(氟离子、甲酸根离子、氯离子、亚硝酸根离子、溴离子、硝酸根离子、硫酸根离子、草酸根离子和磷酸根离子)含量的离子色谱法。方法采用 Ion Pac AS11-HC 阴离子交换分析色谱柱,ASRS 300(250 mm ×4 mm)阴离子抑制型电导检测器检测,7~40 mmol·L -1氢氧化钾溶液梯度淋洗20 min,平衡5 min,流速为1.0 mL ·min -1,柱温为35℃,进样量为20μL。结果9种无机阴离子达到良好分离,0.1~10 mg·L -1的线性关系良好,相关系数为0.9990~0.9998,精密度的 RSD 为0.5%~1.7%,重复性的 RSD 为0.8%~2.7%,稳定性的 RSD 为1.1%~2.9%,平均加样回收率为89.18%~106.81%间,RSD 为0.51%~2.73%(n =6),检测限为0.004~0.023 mg·L -1,定量限为0.015~0.018 mg·L -1。结论该方法快速简单,选择性好,灵敏度高,适用于附子理中丸中9种无机阴离子的含量测定。
Objective To establish the method for simultaneous determination of nine inorganic anions (fluoride,formate,chloride,ni-trite,bromide,nitrate,sulfate,radical,oxalate and phosphate)in Fuzi Lizhong Pills by ion chromatography.Methods Nine inorganic anions were determined by anion exchange column Ion Pac AS11-HC (250 mm ×4 mm),and eluted by gradient hydroxide potassium in 7 ~40 mmol·L -1 .The test took 20 min to determine targets and took 5 min to balance column.And the test was identified by sup-pressed conductivity detector ASRS 300 (4 mm)in the rate of 1.0 mL·min -1 ,and determined at the column temperature of 35 ℃and the sampling volume of 20 μL.Results Good resolution can be achieved among the above mentioned nine inorganic anions.The nine inorganic anions showed a good linear relationship in the range of 0.1 ~10 mg·L -1 ,and their linear correlations over the investi-gated concentration were in the range of 0.999 0 ~0.999 8,while RSDs of precision were 0.5% ~1.7%,RSDs of repeatability 0.8%~2.7%,and RSDs of stability 1.1% ~2.9%.The average recoveries were 89.18% ~106.81% with relative standard deviation be-tween 0.51% and 2.73%,respectively.Conclusions The ion chromatography method is fast,simple,well selective,and well sensitive for the assay and quality control of nine inorganic anions in Fuzi Lizhong Pills.
出处
《安徽医药》
CAS
2016年第8期1490-1494,共5页
Anhui Medical and Pharmaceutical Journal