离子色谱法测定液体创可贴中的氮含量

Determination of nitrogen content in liquid bandage by ion chromatography

目的建立离子色谱法检测液体创可贴中氮含量的方法,对液体创可贴中氮含量进行准确定量来衡量液体创可贴中硝化棉的投料量,进而间接衡量液体创可贴的成膜性、硬度、附着力等性能。方法用DIONX ICS-1100离子色谱仪进行检测,色谱柱AS9-HC柱(4 mm×250 mm),淋洗液为5.0 mmol/L对羟基苯甲酸和5.3 mmol/L N,N-二乙基乙醇胺混合液,流速1 mL/min,电导检测器,外标法定量,用不同浓度梯度的亚硝酸根离子对照品和不同浓度梯度的硝酸根离子对照品分别绘制工作曲线,分别分析不同浓度的亚硝酸根离子和硝酸根离子的出峰时间和峰面积,选取A医疗器械厂家的液体创可贴产品为待测样品,最后将待测样品消解后与对照品平行的进行样品处理并检测。结果亚硝酸根离子在浓度2.9998~6.9995μg/mL范围内与峰面积保持良好的线性关系(r=0.9990),检出限为0.14999 g/mL(S/N=3),精密度相对标准偏差(relative standard deviation,RSD)为1􀆰62%(n=5),平均加标回收率为99.9%(n=9);硝酸根离子在浓度1.7015~3.9701μg/mL范围内与峰面积保持良好的线性关系(r=0.9999),检出限为0.08507μg/mL(S/N=3),精密度RSD为1.48%(n=5),平均加标回收率为100.9%(n=9)。最后对测试样本测试的结果进行计算,得出测试样本中氮的平均含量为11.24 mg/g。结论该方法具备良好的线性范围,准确度高、重复性好,样品经过前处理后,不受样品中其他组分的干扰,可用于液体创可贴中氮含量的测定。

Objective To establish a method for determination of nitrogen content in liquid bandage by Ion Chromatography.The nitrogen content in the liquid bandage was accurately quantified to measure the amount of nitrocotton in the liquid bandage,and then the film formation,hardness,adhesion and other properties of the liquid bandage were indirectly measured.MethodsDIONX ICS-1100 ion chromatograph equipped with AS9-HC column(4 mm×250 mm)and a conductivity detector was used to detect.The eluant was mixture of 5.LN,N-diethylethanolamine with flow rate 1 mL quantified by external standard method.With different concentration gradient of nitrite ion concentration gradient of the reference substance and the different of nitrate ions working curve drawing reference substance respectively,analyzed the different concentrations of nitrite ion and nitrate ion peak time and peak area,selected A bandage products for medical equipment manufacturer liquid sample under test,the final would be under test sample digestion with reference substance after parallel sample processing and testing.ResultsThe linear range of NO2-was 2.9998μg/mL to 6.9995μg/mL(r=09990).The limit of quantitation was 014999μg/mL(S/N=3).The precision RSD was 162%(n=5).And the average recovery was 999%(n=9).The linear range of NO3-was 17015μg/mL to 39701μg/mL(r=09999).The limit of quantitation was 008507μg/mL(S/N=3)The precision RSD was 148%(n=5).And the average recovery was 1009%(n=9).The average/g.Conclusions The method has good linear range,high accuracy and good repeatability.The sample is not disturbed by the other components in the sample after the sample is treated.Therefore the method can be used for the determination of nitrogen content in liquid bandage.