QuEChERS-气相色谱串联质谱法测定茶叶中甲氧滴滴涕残留量

基于一种QuEChERS结合气相色谱串联质谱的方法,测定茶叶中甲氧滴滴涕的残留量,样品中甲氧滴滴涕采用QuEChERS(quick, easy, cheap, effective, rugged, safe)前处理方法,用乙腈提取,试剂盒净化,动态多反映监测(DMRM)扫描,内标法以及基质匹配校准曲线精准定量,在0.01～0.20μg/mL线性范围内,相关系数值R²=0.99902,精密度(RSD)在2.0%～7.9%之间,回收率在80.2%～90.1%之间。该方法省时省力,重现性好,线性范围宽,具有良好的灵敏度和准确度,适用于茶叶中农药多残留的检测分析。     

气相色谱/质谱法测定饮用水中挥发性有机物

建立了吹扫捕集与气相色谱一质谱联用测定饮用水中13种挥发性有机物的分析方法．该方法的加标回收率在90％～110％之间，相对标准偏差基本小于5．0％，该方法灵敏度高、准确度好，已成功地用于饮用水中挥发性有机污染物的测定，结果令人满意．     

电感耦合等离子质谱法测定地质样品中的稀贵金属元素

研究建立了直接用王水消解地质勘探样品，利用电感耦合等离子质谱仪(ICP—MS测定其中稀贵金属元素Au、Pt、Pd、Ir、Ru、Rh的分析方法,建立校正方程及引入内标元素Cs，有效克服了质谱干扰及由于基体效应产生的非质谱干扰．方法的测定下限为0．7—2．0ng/g，精密度为3．3％-7．4％，加标回收率为91％-113％，适于大量地质样品中稀贵金属元素的及时分析。     

气相色谱-四极杆飞行时间质谱法同时测定水产品中19种多氯联苯

建立同时测定水产品中19种多氯联苯的气相色谱-四级杆飞行时间质谱法。样品采用丙酮和石油醚混合溶液为提取溶剂,利用分散高速匀质法提取19种多氯联苯,提取液用浓硫酸和层析柱进行双重净化,正己烷洗脱,经气相毛细管柱(HP-5MS)分离,以1.5mL/min流速的氦气作为载气,电子轰击离子源电离,用TOF/MS全扫描模式采集数据,以保留时间和离子精确质量数定性,外标法定量,建立了水产品中19种多氯联苯同时测定的方法。结果显示19种多氯联苯在5.0~500.0μg/L线性良好,相关系数大于0.9986,方法检出限(LOD,S/N=3)介于0.12~1.07μg/kg,方法定量限(LOQ,S/N=10)介于0.40 ~3.57μg/kg。在5.0,10.0,20.0μg/kg 3种加标水平下,19种多氯联苯的平均回收率介于79.6%~103.4%,日内相对标准偏差介于2.2%~9.6%；在20.0,100.0,200.0μg/kg 3种加标水平下,19种多氯联苯的平均回收率介于77.4%~104.6%,日间相对标准偏差介于2.7%~9.8%。结果表明,建立的检测方法准确、灵敏、可靠,可用于水产品中19种多氯联苯的监督检测。     

同位素内标法对水产品中硝基呋喃代谢物液相色谱-串联质谱法测定

建立了水产品中硝基呋喃类代谢物残留量的同位素内标定量液相色谱-串联质谱法测定。样品经稀盐酸水解,邻硝基苯甲醛衍生,乙酸乙酯提取净化后,用液相色谱-串联质谱法通过正离子扫描多反应监测模式检测,稳定同位素内标定量。本方法的线性范围为1.25～10μg/kg,4种硝基呋喃代谢物的线性相关系数均在0.993 2以上,4种化合物...     

A gas chromatography/mass spectrometry method for the simultaneous analysis of 50 phenols in wastewater using deconvolution technology

Phenolic compounds exist widely in the influents and effluents of sewage treatment plants (STPs) and most are un-regulated. In this study, a gas chromatography-mass spectrometry (GC-MS) method for the simultaneous analysis of 50 phenolic compounds in wastewater was developed. Deconvolution technology was used to identify contaminants that are covered by co-extracted materials. A mass spectral library containing all 50 silylated phenolic compounds was first established and used for deconvolution. Twelve typical phenolic compounds were selected to optimize the sample preparation procedures. Solid-phase extraction using a C18 cartridge coupled with an HLB cartridge was used for pre-concentration and dichloromethane was used for elution. The solutes were derivatized and analyzed by GC-MS. The blank and matrix spike recoveries ranged from 57.46% to 136.4% and 47.87% to 114.8%, respectively. Method detection limits ranged from 3.64 to 97.64 ng L⁻¹. The relative standard deviations of all the recovery experiments were lower than 13.6%. The instrument limits of quantification ranged from 0.7 to 87.7 pg. The method has been applied to analyze the influents and effluents of 5 Chinese STPs. Except for regulated phenolic compounds (phenol and 2,4,6-trichlorophenol), three un-regulated phenolic compounds, including 2-chlorophenol, 2,5-dichlorophenol and 2,4-dichloro-3-ethyl-6-nitrophenol were identified in the effluent wastewater. The detected concentrations of un-regulated phenolic compounds could possibly cause environmental effects, indicating that immediate attention is required to prevent complications.     

气相色谱-质谱法分析无籽罗汉果果实中挥发油成分

采用水蒸气蒸馏法提取无籽罗汉果果实中的挥发油,经气相色谱-质谱联机分析,鉴定出挥发油中的24个化学成分.其主要成分为:乙二醇异丙醚(27.21%)、1,2-苯二甲酸丁基-2-乙基己酯(13.51%)、邻苯二甲酸二异丁酯(10.85%)、天竺葵醛(10.22%)、(E)3-癸烯酸(6.52%)、丁酸丁酯(4.99%)、乙...     

阿托品肝匀浆代谢物的液相色谱-串联质谱法检测

运用液相色谱-电喷雾离子阱串联质谱(LC-MSn)联用技术分析检测阿托品大鼠肝匀浆中的代谢物.采用离体实验的代谢研究方法,将阿托品与大鼠肝匀浆在富氧条件下温孵,代谢物以乙酸乙酯萃取,采用LC-MS及LC-MSn等方法进行分析.和原药相比较,根据温孵液中分析物分子量的变化(ΔM)及其多级质谱数据,鉴定代谢物并阐述其结构.结果在阿托品的大鼠肝匀浆培养液中发现了脱水阿托品和去甲基阿托品2种代谢物.     

超临界CO2萃取法提取库尔勒香梨精油及其成分分析研究

采用超临界CO2萃取法提取库尔勒香梨精油,用气相色谱-串联质谱技术对其成分进行分析,并对几种提取方法进行综合比较。结果表明,与水蒸气蒸馏法、固相微萃取法相比,超临界CO2萃取法具有香梨精油提取率最高,为0．0549％。感官分析的结果表明,超临界CO2萃取法所得的库尔勒香梨精油颜色为橙色透明液体,而且风味好。气相色谱-质谱联用（GC-MS）分析结果表明：超临界CO2萃取法所得的香梨精油中共鉴定出28种成分。丁酸乙酯、顺-7-十四烯-1-醇和乙酸己酯的含量最高,含量分别为5．19％、4．85％和4．37％。