离子色谱法同时测定附子理中丸中9种无机阴离子含量

摘要

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.%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。