北京生物醫(yī)學(xué)工程

離子色譜法測(cè)定液體創(chuàng)可貼中的氮含量

Determination of nitrogen content in liquid bandage by ion chromatography

作者：崔永平林紅賽黃永富王利霞岳衛(wèi)華

單位：北京市醫(yī)療器械檢驗(yàn)所(北京 101111)

關(guān)鍵詞：液體創(chuàng)可貼; 氮含量; 離子色譜

分類號(hào)：R318

出版年·卷·期（頁(yè)碼）：2020·39·1（86-91）

摘要：

目的建立離子色譜法檢測(cè)液體創(chuàng)可貼中氮含量的方法，對(duì)液體創(chuàng)可貼中氮含量進(jìn)行準(zhǔn)確定量來(lái)衡量液體創(chuàng)可貼中硝化棉的投料量，進(jìn)而間接衡量液體創(chuàng)可貼的成膜性、硬度、附著力等性能。方法用DIONX ICS-1100離子色譜儀進(jìn)行檢測(cè)，色譜柱AS9-HC柱（4 mm×250 mm），淋洗液為5.0 mmol/L對(duì)羥基苯甲酸和5.3 mmol/L N,N-二乙基乙醇胺混合液，流速1 mL/min，電導(dǎo)檢測(cè)器，外標(biāo)法定量，用不同濃度梯度的亞硝酸根離子對(duì)照品和不同濃度梯度的硝酸根離子對(duì)照品分別繪制工作曲線，分別分析不同濃度的亞硝酸根離子和硝酸根離子的出峰時(shí)間和峰面積，選取A醫(yī)療器械廠家的液體創(chuàng)可貼產(chǎn)品為待測(cè)樣品，最后將待測(cè)樣品消解后與對(duì)照品平行的進(jìn)行樣品處理并檢測(cè)。結(jié)果亞硝酸根離子在濃度2.999 8~6.999 5 mg/mL范圍內(nèi)與峰面積保持良好的線性關(guān)系（r=0.999 0），檢出限為0.149 99 mg/mL（S/N=3），精密度RSD：1.62%（n=5），平均加標(biāo)回收率為99.9%（n=9）；硝酸根離子在濃度1.7015~3.9701 mg/mL范圍內(nèi)與峰面積保持良好的線性關(guān)系（r=0.9999），檢出限為0.085 07 mg/mL（S/N=3），精密度RSD：1.48%（（n=5），平均加標(biāo)回收率為100.9%（n=9），最后對(duì)測(cè)試樣本測(cè)試的結(jié)果進(jìn)行計(jì)算得出測(cè)試樣本中氮的平均含量為11.24 mg/g。結(jié)論該方法具備良好的線性范圍、準(zhǔn)確度高、重復(fù)性好，樣品經(jīng)過(guò)前處理后，不受樣品中其他組分的干擾，可用于液體創(chuàng)可貼中氮含量的測(cè)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. Methods DIONX 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 5.0mmol/L phydroxybenzoic acid and 5.3mmol/L N,N-Diethylethanolamine with flow rate 1mL/min. and 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. Results The linear range of NO2- was 2.999 8 mg/mL to 6.999 5 mg/mL(r=0.999 0). The limit of quantitation was 0.149 99mg/mL（S/N=3）.The precision RSD was 1.62% (n=5). And the average recovery was 99.9% (n=9). The linear range of NO3- was 1.701 5 mg/mL to 3.970 1 mg/mL (r=0.999 9).The limit of quantitation was 0.08507mg/mL（S/N=3）The precision RSD was 1.48%（n=5）. And the average recovery was 100.9%（n=9）. The average nitrogen content in the test sample was 11.24 mg/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.

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