离子色谱法测定明目上清片中常见无机阴离子含量

Determination of common inorganic anions in mingmushangqing tablets by ion chromatography

目的建立同时测定明目上清片中9种常见无机阴离子含量的离子色谱法。方法采用改进的QuEChERS前处理方法净化样品,离子色谱法测定样品。用去离子水提取,N-丙基乙二胺(PSA)和C_(18)净化,Ion Pac AS11-HC阴离子交换分析柱分离,氢氧化钾淋洗液梯度洗脱,洗脱25 min,流速为1.0 mL·min^(-1),柱温为30℃,进样量为30μL。结果 9种常见无机阴离子均能达到基线分离,线性范围在0.5~50.0 mg·L^(-1)之间,线性关系良好,相关系数为0.999 0~0.999 9范围内,仪器精密度、重复性和稳定性良好,平均加样回收率为90.26%~101.22%,RSD为0.51%~2.15%,仪器精密度、重复性和稳定性良好。结论该方法简便快速和自动化,可用于明目上清片中无机阴离子含量的测定。

Objective To establish the method for simultaneous determination of common inorganic anions （ fluoride, formate, chloride, nitrite, bromide, nitrate, sulfate, oxalate and phosphate ） in Mingmushangqing tablets by ion chromatograph. Method The samples were extracted by using Quick,Easy,Cheap, Effective, Rugged and Safe extraction （QuEChERS） and determined by ion chromatography. Common inorganic anions were determined by anion exchange column Ion Pac AS11-HC and eluted for 25 min by gradient hydroxide potassium in at the rate of 1.0 mL·min-1 and the temperature of 30 ,and the sampling volume was 30 jjlL. Results Good resolu-tion can be achieved among the above mentioned nine inorganic anions. The nine inorganic anions showed a good linear relationship in the ranges of 0. 5- 50. 0 mg·L-1 and their linear correlations over the investigated concentration were in the range of 0. 999 0- 0. 999 9,while relative standard deviations,repeatability and stability were good. The average recoveries were 90.26% -101.22% with rela-tive standard deviation of 0. 51% - 2. 15% respectively. Conclusion The ion chromatography method were the better simple, fast and automated for determine nine inorganic anions in mingmushangqing tablets.