加速溶剂萃取-离子色谱法同时测定黄连上清片中9种常见无机阴离子的含量 点击下载
论文标题: 加速溶剂萃取-离子色谱法同时测定黄连上清片中9种常见无机阴离子的含量
英文标题:
中文摘要: 目的:建立同时测定黄连上清片中9种常见无机阴离子含量的方法。方法:采用加速溶剂萃取-离子色谱法。阴离子交换分析柱为Ion Pac AS11-HC,保护柱为Ion Pac AG11-HC,淋洗液为氢氧化钾溶液(梯度洗脱),流速为1.2 mL/min,洗脱时间为18 min,柱温为30 ℃,进样体积为25 μL。结果: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检测质量浓度线性范围均为0.1~5 mg/L(r为0.999 0~0.999 9);定量限分别为0.020、0.078、0.030、0.058、0.052、0.068、0.084、0.064、0.074 mg/L,检测限分别为0.005、0.024、0.008、0.017、0.015、0.022、0.026、0.020、0.021 mg/L;精密度、稳定性、重复性试验的RSD<4.0%;加样回收率为80.00%~125.08%(RSD为0.97%~2.47%)。结论:该方法操作简便,精密度、稳定性、重复性好,可用于黄连上清片中9种常见无机阴离子含量的同时测定。
英文摘要: OBJECTIVE:To establish the method for simultaneous determination of 9 common inorganic anions in Huanglian shangqing tablet. METHODS:The accelerated solvent extraction-ion chromatography was adopted. Inorganic anions were determined by Ion Pac AS11-HC anion exchange column, protected by Ion Pac AG11-HC column and eluted by hydroxide potassium solution (gradient elution) at the flow rate of 1.2 mL/min. The column temperature was set at 30 ℃, elution time was 18 min, and sample volume was 25 mL. RESULTS: The linear ranges of fluorinion, formate ion, nitrite ion, bromide ion, nitrate ion, sulfate ion, oxalate ion and phosphate ion were 0.1-5 mg/L(r=0.999 0-0.999 9). The limits of quantitation were 0.020, 0.078, 0.030, 0.058, 0.052, 0.068, 0.084, 0.064, 0.074 mg/L, and the limits of detection were 0.005, 0.024, 0.008, 0.017, 0.015, 0.022, 0.026, 0.020, 0.021 mg/L, respectively. RSDs of precision, stability and repeatability were all lower than 4.0%; recoveries were 80.00%-125.08% (RSD ranged 0.97%-2.47%). CONCLUSIONS: The method is simple, precise, stable and repeatable, and can be used for 9 common inorganic anions in Huanglian shangqing tablet.
期刊: 2017年第28卷第12期
作者: 胡恩泽,魏明,黄正辉
英文作者: HU Enze,WEI Ming,HUANG Zhenghui
关键字: 加速溶剂萃取;离子色谱法;黄连上清片;无机阴离子
KEYWORDS: Accelerated solvent extraction; Ion chromatography; Huanglian shangqing tablet; Inorganic anion
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