GC-MS法同时测定橡皮擦中22种邻苯二甲酸酯增塑剂

建立了气相色谱-质谱(GC-MS)分段选择离子监测(SIM)模式分析同时测定橡皮擦中22种邻苯二甲酸酯(PAEs)增塑剂含量的方法。该方法具有良好线性,相关系数R均大于0.999,检测限在1.3 mg/kg～128.9 mg/kg之间,平均回收率在70.2%～105.6%,相对标准偏差在2.57%～9.88%之间。通过该方法对国内橡皮擦中PAEs增塑剂进行检测,实际样品均检出邻苯二甲酸二(2-乙基)己酯(DEHP),含量最高达32.5%。     

气-质联机对嗪草酮原药及其主要杂质的分析

采用气桐色谱-质谱（GC—MS）联用对嗪草酮原药主成分及主要杂质进行分析,结合嗪草酮原药合成工艺,确定了3个主要杂质的结构和含量。同时利用杂质结构对嗪草酮的合成新方法进行验证。     

用毛细管气相色谱与质谱检测联用技术测定炼油厂中的水中有 …

利用毛细管气相色谱与质谱检测（ＧＣ－ＭＳ）联用技术定性和定量分析中和水中有机污染物,探讨了污水中有机物的富集方法以及ＧＣ－ＭＳ法测定污水中有机物的精度和回收率。结果表明,该方法灵敏度高,线性范围宽,回收率高。     

Stability Studies of Ozonized Sunflower Oil and Enriched Cosmetics with a Dedicated Peroxide Value Determination

Ozonized oils have interesting applications in the cosmetic industry and several patents on enriched products were developed in the last years. Ozonides are known for their high reactivity and stability data are required for enriched cosmetic products during storage. In this paper a dedicated determination of Peroxide Value (PV) was performed on ozonized sunflower oil (Neozone 4000) and on some enriched cosmetics, in order to control their stability during storage. The optimal conditions of the PV method were determined, following the decomposition reaction of ozonides with KI utilizing ¹H-NMR and GC/MS techniques.     

Fast headspace-enantioselective GC-mass spectrometric-multivariate statistical method for routine authentication of flavoured fruit foods

This study describes a rapid total analysis system (TAS) to detect the authenticity of fruit-flavoured foods and beverages by on-line combining headspace solid phase microextraction (HS-SPME) with enantioselective GC-MS (Es-GC-MS) and statistical multivariate methods (PCA, HCA). Peach, coconut, apricot, raspberry, as fruits mainly characterised by γ- and δ-lactones as chiral markers, strawberry (α-ionone, linalool, nerolidol, ethyl 2-methylbutyrate, 2-methylbutyric acid and γ-lactones) and melon (ethyl 2-methylbutyrate and 2-methylbutanol) were investigated. The system was developed by (a) optimising non-equilibrium HS-SPME sample preparation, (b) speeding-up ES-GC using cyclodextrin derivatives as chiral selectors with conventional and narrow-bore columns and (c) elaborating data by multivariate methods. The resulting TAS affords a reduction of the time needed for the whole analytical process from about 150 min to 20-50 min (67-87% of the current routine method) depending on matrix, sampling and analysis conditions and Es-GC columns.     

气质联用法测定电视外壳中十种多溴二苯醚

建立了电视机外壳样品中10种多溴二苯醚的微波萃取-气质联用测定方法。10种多溴二苯醚的定量峰面积与其浓度在一定范围内成线性关系,检出限从0.08μg/m L到0.60μg/m L。采用索氏萃取法进行方法验证,测试结果的RSD≤2.83,两种方法经t检验无显著性差异。该方法具有简便、快速、试剂消耗量少的优点,可应用于电视机等国推污染控制认证产品塑料材料中多溴二苯醚测定。     

吸附剂针对性净化-气相色谱-三重四极杆串联质谱测定油茶果中55种持久性有机污染物

建立了针对性净化与气相色谱-串联质谱相结合的方法,测定油茶果不同部位中16种多环芳烃、18种多氯联苯和21种有机氯共55种持久性有机污染物（POPs）。油茶籽仁、油茶外种皮和油茶壳样品采用乙腈提取,氯化钠盐析,离心分层后,分别向提取液中加入无水硫酸镁和PSA、C18、Florisil、Si、SCX、NANO Carb与Pesticarb等 7种吸附剂进行多管漩涡振荡分散固相净化比较,多反应监测模式检测。结果表明,55种持久性有机污染物在20~1 000 μg/L浓度范围内具有良好的线性关系,检出限为0.25~65.50 μg/kg,定量限为0.84~218.34 μg/kg,加标回收率为69.1%~138.2%。应用本方法检测来自湖南、江西和浙江共54份油茶的POPs,从油茶籽仁检出萘、狄氏剂、芴、毒杀芬、菲、α-六六六和苊萘嵌戊烷（4.36~566.26 μg/kg）;外种皮检出萘、芴、菲、毒杀芬、α-六六六和苊萘嵌戊烷（3.62~1 109.43 μg/kg）;油茶壳检出萘、毒杀芬、芴和菲（5.13~703.57 μg/kg）。该方法适用于油茶果不同部位持久性有机污染物的检测,对其他油料作物的POPs分析也具有一定的参考价值。     

基于特征性离子快速筛查和识别色胺类新精神活性物质

采用气相色谱-质谱(GC-MS)法和超高效液相色谱-串联四极杆飞行时间质谱(UPLC-QTOF MS)法分析2015~2019年国内检测发现的11种色胺类新精神活性物质。GC-MS在电子轰击源(EI)模式下采集数据,UPLC-QTOF MS在电喷雾正离子(ESI⁺)-碰撞诱导解离(CID)模式下采集数据。通过对目标物质谱裂解产生的特征性离子进行分析,推测了色胺类新精神活性物质可能的碎裂途径,建立了一种快速、便捷筛查和识别色胺类新精神活性物质的方法。     

Optimization of supercritical CO2 extraction of dried Helichrysum italicum flowers by response surface methodology: GC-MS profiles of the extracts and essential oil

Supercritical (SC) CO₂ extraction of dried Immortelle flowers was performed at different process parameters. The optimal extraction conditions related to the yield were determined by response surface methodology (yield 4.09% at 20 MPa and 52°C). The extracts were analyzed by GC-MS and tremetone derivatives dominated: bitalin A, 12-acetoxytremetone, gnaphaliol, 1-[2-(2-methyl-2,3-dihydroxypropyl)-2,3-dihydro-1-benzofuran-5-yl]ethanone, isobutyl bitalin A, and 1-[2-(acetylprop-1-en-2-yl)-3-hydroxy-2,3-dihydro-1-benzofuran-5-yl]ethanone. Striking differences were found among the essential oil and SC-CO₂ extracts composition. The major oil compounds were γ-curcumene, α-pinene, β-selinene, α-selinene, and limonene. Mono- and sesquiterpene were found among minor constituents of the extracts. Neryl acetate was present in the extracts and essential oil.     

GPC净化联合GC-MS/MS测定番石榴中2种杀菌剂残留

建立同时测定番石榴中三唑酮和腐霉利的气相色谱-串联质谱(GC-MS/MS)分析方法。番石榴样品经乙腈提取,凝胶渗透色谱净化,GC-MS/MS检测,外标法定量。结果表明:三唑酮和腐霉利在0.05~0.50 mg/kg范围内,回收率在77.4%~100.7%之间,相对标准偏差为5.0%~9.6%(n=5)。三唑酮、腐霉利定量限分别为0.01和0.005 mg/kg。该方法灵敏、准确,适用于番石榴中2种杀菌剂的残留检测分析。