分析测试学报
分析測試學報
분석측시학보
JOURNAL OF INSTRUMENTAL ANALYSIS
2010年
1期
26-30
,共5页
朱文静%杨俊%刘百战%苏庆德%陆怡峰%周宛虹
硃文靜%楊俊%劉百戰%囌慶德%陸怡峰%週宛虹
주문정%양준%류백전%소경덕%륙이봉%주완홍
超高效液相色谱-串联质谱%烟草特有亚硝胺%卷烟烟气%固相萃取
超高效液相色譜-串聯質譜%煙草特有亞硝胺%捲煙煙氣%固相萃取
초고효액상색보-천련질보%연초특유아초알%권연연기%고상췌취
UPLC-MS/MS%tobacco-specific nitrosamines(TSNAs)%mainstream cigarette smoke%solid phase extraction
建立了卷烟主流烟气中烟草特有亚硝胺的超高效液相色谱-电喷雾串联质谱(UPLC-MS/MS)测定方法.在标准吸烟条件下,采用剑桥滤片收集卷烟烟气粒相物,用醋酸铵缓冲液提取粒相物,经固相萃取净化后,以电喷雾正离子多反应监测方式,实现了烟气中N-亚硝基降烟碱、4-甲基亚硝基吡啶基丁酮、N-亚硝基新烟草碱和N-亚硝基假木贼碱的基线分离和快速测定.4种烟草特有亚硝胺在0 ~400 μg/L范围内具有良好线性,相关系数大于0.998,定量下限为0.08 ~0.15 μg/L,加标回收率为72% ~104%,相对标准偏差为3.8% ~9.7%.该方法灵敏、快速、准确,适用于卷烟烟气中烟草特有亚硝胺的测定.
建立瞭捲煙主流煙氣中煙草特有亞硝胺的超高效液相色譜-電噴霧串聯質譜(UPLC-MS/MS)測定方法.在標準吸煙條件下,採用劍橋濾片收集捲煙煙氣粒相物,用醋痠銨緩遲液提取粒相物,經固相萃取淨化後,以電噴霧正離子多反應鑑測方式,實現瞭煙氣中N-亞硝基降煙堿、4-甲基亞硝基吡啶基丁酮、N-亞硝基新煙草堿和N-亞硝基假木賊堿的基線分離和快速測定.4種煙草特有亞硝胺在0 ~400 μg/L範圍內具有良好線性,相關繫數大于0.998,定量下限為0.08 ~0.15 μg/L,加標迴收率為72% ~104%,相對標準偏差為3.8% ~9.7%.該方法靈敏、快速、準確,適用于捲煙煙氣中煙草特有亞硝胺的測定.
건립료권연주류연기중연초특유아초알적초고효액상색보-전분무천련질보(UPLC-MS/MS)측정방법.재표준흡연조건하,채용검교려편수집권연연기립상물,용작산안완충액제취립상물,경고상췌취정화후,이전분무정리자다반응감측방식,실현료연기중N-아초기강연감、4-갑기아초기필정기정동、N-아초기신연초감화N-아초기가목적감적기선분리화쾌속측정.4충연초특유아초알재0 ~400 μg/L범위내구유량호선성,상관계수대우0.998,정량하한위0.08 ~0.15 μg/L,가표회수솔위72% ~104%,상대표준편차위3.8% ~9.7%.해방법령민、쾌속、준학,괄용우권연연기중연초특유아초알적측정.
A specific and sensitive method had been developed to rapidly separate and determine 4 tobacco-specific nitrosamines(TSNAs),including N'-nitrosonornicotine(NNN),4-(N-methylnitrosamino)-1-(3-pyridyl)-1-butanone(NNK),N'-nitrosoanatabine(NAT) and N'-nitrosoanabasine(NAB),in mainstream cigarettes smoke by employing ultra-performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS).Total particulate matters in mainstream smoke were trapped by cambridge filter pad under standard smoking condition,extracted by using ammonium acetate buffer as solvent,cleaned up on solid phase extraction(SPE),and then analyzed by UPLC-MS/MS with positive electrospray ionization(ESI) under multiple reaction monitoring(MRM) mode.The supersonic extraction time,experimental conditions of UPLC and MS were also optimized.Under the optimal conditions,the calibration curves showed good linearity for 4 TSNAs in the concentration ranges of 0-400 μg/L with correlation coefficients above 0.998.The limits of quantitation(LOQ) were between 0.08 and 0.15 μg/L(S/N=10),and average recoveries ranged from 72% to 104% with RSDs of 3.8%-9.7%.The method was sensitive,rapid and accurate,and was suitable for the determination of TSNAs in mainstream cigarette smoke.