化学分析计量
化學分析計量
화학분석계량
CHEMICAL ANALYSIS AND METERAGE
2015年
1期
28-32
,共5页
于小焱%张晓慧%庞永超
于小焱%張曉慧%龐永超
우소염%장효혜%방영초
凝胶排阻色谱%聚乙二醇%截留率%中空纤维超滤膜组件%相对分子质量
凝膠排阻色譜%聚乙二醇%截留率%中空纖維超濾膜組件%相對分子質量
응효배조색보%취을이순%절류솔%중공섬유초려막조건%상대분자질량
size exclusion chromatography%polyethylene glycol%retention rate%hollow fiber ultrafiltration membrane module%relative molecular mass
采用凝胶排阻色谱法测定中空纤维超滤膜组件对聚乙二醇20000(PEG20000)溶液的截留率,选择Agilent PL aquagel-OH MIEXD–H8μm色谱柱,流动相为0.1 mol/L NaNO3溶液(含0.02%NaN3),流量为1 mL/min,RID检测器,柱温箱和检测器温度均为30℃。当进样体积为50μL时,方法的检出限为18.8 mg/L,定量限为49.0 mg/L。PEG20000溶液的质量浓度在60~1000 mg/L范围内与色谱峰高呈良好的线性,相关系数r2=1.000。该方法对实际样品测定结果的相对标准差为1.31%(n=6)。将该方法的测定结果与紫外–可见分光光度计法的测量结果进行F检验和t检验,结果表明两种方法测量结果无显著性差异。采用该方法可以同时对PEG20000样品的相对分子质量及其分布进行测定,从而对选用的截留标准物质进行质量控制。
採用凝膠排阻色譜法測定中空纖維超濾膜組件對聚乙二醇20000(PEG20000)溶液的截留率,選擇Agilent PL aquagel-OH MIEXD–H8μm色譜柱,流動相為0.1 mol/L NaNO3溶液(含0.02%NaN3),流量為1 mL/min,RID檢測器,柱溫箱和檢測器溫度均為30℃。噹進樣體積為50μL時,方法的檢齣限為18.8 mg/L,定量限為49.0 mg/L。PEG20000溶液的質量濃度在60~1000 mg/L範圍內與色譜峰高呈良好的線性,相關繫數r2=1.000。該方法對實際樣品測定結果的相對標準差為1.31%(n=6)。將該方法的測定結果與紫外–可見分光光度計法的測量結果進行F檢驗和t檢驗,結果錶明兩種方法測量結果無顯著性差異。採用該方法可以同時對PEG20000樣品的相對分子質量及其分佈進行測定,從而對選用的截留標準物質進行質量控製。
채용응효배조색보법측정중공섬유초려막조건대취을이순20000(PEG20000)용액적절류솔,선택Agilent PL aquagel-OH MIEXD–H8μm색보주,류동상위0.1 mol/L NaNO3용액(함0.02%NaN3),류량위1 mL/min,RID검측기,주온상화검측기온도균위30℃。당진양체적위50μL시,방법적검출한위18.8 mg/L,정량한위49.0 mg/L。PEG20000용액적질량농도재60~1000 mg/L범위내여색보봉고정량호적선성,상관계수r2=1.000。해방법대실제양품측정결과적상대표준차위1.31%(n=6)。장해방법적측정결과여자외–가견분광광도계법적측량결과진행F검험화t검험,결과표명량충방법측량결과무현저성차이。채용해방법가이동시대PEG20000양품적상대분자질량급기분포진행측정,종이대선용적절류표준물질진행질량공제。
The method for determining polyethylene glycol (PEG)retention rate of hollow fiber ultrafiltration membrane module by high performance size exclusion chromatography (SEC) was established. An Agilent PL aquagel-OH MIEXD–H 8 μm column was used,and the chromatographic conditions were as follows: the mobile phase was 0.1 mol/L NaNO3 solution (with 0.02% NaN3) with flow rate of 1 mL/min,RID detector was selected and the temperature of the column and detector was 30℃. The detection limit of the method was 18.8 mg/L and quantification limit was 49.0 mg/L as single injection volume was 50μL. The concentration of PEG20000 was linear with peak height in the range of 60–1 000 mg/L and the linear correlation coefficient(r2) was 1.000. The relative standard deviation of sample detection results was 1.31%. The detection results of the method had no significant difference compared with traditional visible spectrophotometry by t-Test and F-test. The method can be used for determining relative molecular mass and its distribution simultaneously,and controlling the quality of the retention test standard materials (PEGs).