广州化工
廣州化工
엄주화공
GUANGZHOU CHEMICAL INDUSTRY AND TECHNOLOGY
2015年
8期
140-143
,共4页
N-甲基吡咯烷酮%PU革%超声提取%固相萃取%气相色谱-质谱法
N-甲基吡咯烷酮%PU革%超聲提取%固相萃取%氣相色譜-質譜法
N-갑기필각완동%PU혁%초성제취%고상췌취%기상색보-질보법
1-methyl-2-pyrrolidinone%poly urethane leather%ultrasonic extraction%solid phase extraction%gas chromatography-mass spectrometry
结合超声波提取、固相萃取小柱（ SPE）净化的前处理技术，建立气相色谱－质谱法（ GC－MS）快速检测PU革中N－甲基吡咯烷酮（ NMP）残留量方法。考察了影响样品前处理因素显示，室温下以丙酮为提取剂超声提取30 min可以较完全地提取PU革中NMP，以3砄2混合的活性炭与Florisil硅藻土为吸附剂SPE柱和正己烷＋乙酸乙酯（V／V＝1／20）混合溶剂为洗脱液可以较好洗脱、净化提取液中NMP，以SCAN／SIM同时检测扫描（ FASST）模式分析试液，外标法定量。结果表明， NMP浓度在线性范围内的回收率94％～101.3％，相对标准偏差RSD（n＝5）6.5％～1.3％，定量限0.0457 mg· kg－1。本方法操作简单、快速、准确，灵敏度高，重现性好，可满足PU革中NMP残留量检测的日常要求。
結閤超聲波提取、固相萃取小柱（ SPE）淨化的前處理技術，建立氣相色譜－質譜法（ GC－MS）快速檢測PU革中N－甲基吡咯烷酮（ NMP）殘留量方法。攷察瞭影響樣品前處理因素顯示，室溫下以丙酮為提取劑超聲提取30 min可以較完全地提取PU革中NMP，以3砄2混閤的活性炭與Florisil硅藻土為吸附劑SPE柱和正己烷＋乙痠乙酯（V／V＝1／20）混閤溶劑為洗脫液可以較好洗脫、淨化提取液中NMP，以SCAN／SIM同時檢測掃描（ FASST）模式分析試液，外標法定量。結果錶明， NMP濃度在線性範圍內的迴收率94％～101.3％，相對標準偏差RSD（n＝5）6.5％～1.3％，定量限0.0457 mg· kg－1。本方法操作簡單、快速、準確，靈敏度高，重現性好，可滿足PU革中NMP殘留量檢測的日常要求。
결합초성파제취、고상췌취소주（ SPE）정화적전처리기술，건립기상색보－질보법（ GC－MS）쾌속검측PU혁중N－갑기필각완동（ NMP）잔류량방법。고찰료영향양품전처리인소현시，실온하이병동위제취제초성제취30 min가이교완전지제취PU혁중NMP，이3결2혼합적활성탄여Florisil규조토위흡부제SPE주화정기완＋을산을지（V／V＝1／20）혼합용제위세탈액가이교호세탈、정화제취액중NMP，이SCAN／SIM동시검측소묘（ FASST）모식분석시액，외표법정량。결과표명， NMP농도재선성범위내적회수솔94％～101.3％，상대표준편차RSD（n＝5）6.5％～1.3％，정량한0.0457 mg· kg－1。본방법조작간단、쾌속、준학，령민도고，중현성호，가만족PU혁중NMP잔류량검측적일상요구。
A method for rapid determination of 1-methyl-2-pyrrolidinone residues in poly urethane ( PU) leather was developed by gas chromatography-mass spectrometry after pre-treatment processes of ultrasonic-assisted extraction and solid phase extraction ( SPE ) decontamination.The factors that effected the pretreatment of samples were investigated.The results showed that NMP residues in PU leather were extracted more completely for 30 min employing acetone as extracting agent with ultrasonic assisted at room temperature, cleaned-up through the SPE cartridge filled with activated carbon and florisil diatomite (3:2) as adsorbent and eluted with n-hexane and ethyl acetate (V/V=1/20) mixture.The test solutions were analyzed by GC-EI/MS and Fast Automated Scan/SIM Type ( FASST) model.The data was identified and quantified with the exterior standard method.The results showed that the limit of quantification was 0.0457 mg · kg-1 .The recoveries were between 94% and 101.30%, and the relative standard deviations were from 6.5%to 1.3%.These results suggested that the developed method was simple, rapid, accurate and highly sensitive, and can meet daily testing requirements of NMP residues in PU leather.
