毛竹保健功能成分的GC／MS分析

采用混合溶剂萃取法从新鲜毛竹片中提取成分，浓缩后，利用GC／MS联机分析技术，用色谱峰面积归一化法计算各组分的相对含量。共分离出66个峰，结合文献调研，鉴定出52个化合物，占总峰面积的99．36％。主要成分为维生素E（13．18％）、十六酸（8．95％）、（z，z）-9，12-十八碳二烯酸（8、15％）、十二烷（6．19％）、十三烷（5．44％）、2，6，10-甲基-十四烷（4．86％）、1H-吲哚（4．49％）、羽扇豆醇（3．84％）、驱蚊叮（3．83％）、氧代-12-烯-24-羧酸，3-氧络-甲酯（＋）-（3、67％）、（3á）-豆甾-5-烯-3-醇（3．06％）、十一烷（2．96％）、二十七烷（2．92％）、十九烷（2．51％）、十四烷（2．45％）、十五烷（2．08％）、十六烷（2．19％）、（z）-9-十八碳烯酸（2．12％）、亚油酸乙酯（1．95％）、1,2-邻苯二甲酸二异辛酯（1．75％）、二十五烷（1．63％）、二十一烷（1．18％）、1,2-苯二甲酸双（2-甲丙基）酯（1．02％）等．以上成分中，大部分具有天然保健功效，且含量较高，由此可见，毛竹中富含保健功能的天然成分．     

南竹过热水萃取物成分的GC／MS分析

在新鲜南竹片过热水萃取物GC／MS分析中，共分离出36个峰，结合文献调研，鉴定出25个化合物，占总峰面积的97．35％．主要成分为二十七烷（cas）（26．2％）、14-á-H-pregna（15．71％）、2，6，10-甲基-十四烷（15．55％）、甲基-9，10-二氟次甲基-9-十八碳二烯酸（12．84％）、1，2-邻苯二甲酸二丁基酯）（8．93％）、1，2-邻苯二甲酸，双2-甲丙酯（2．65％）、1-五十七醇（1．88％）、isochiapin b（％1．88）、10-甲氧基-nb-à-甲基二十九醇（1．63％）等．     

不同产地黑老虎挥发油成分的GC-MS分析研究

采用水蒸气蒸馏法,GC-MS分离检测技术,分析研究了福建、广西、广东三个不同产地黑老虎挥发油的成分。共鉴定出51种化合物,挥发油总量福建占77.82%,广西占78.62%,广东占78.83%。其中有20种为共有成分,主要包括δ-荜澄茄烯、β-石竹烯、α-可巴烯、葎草烯、别香橙烯、γ-衣兰油烯等,分别占各自挥发油总量的51.45%(福建),38.08%(广西),62.95%(广东)。结果表明,不同产地黑老虎挥发油含量及化学成分组成差异较大。     

生姜与生姜皮挥发油成分的分析

目的：定性定量分析生姜与生姜皮挥发油成分。方法：利用气相色谱-质谱法分离检测生姜与生姜皮挥发油成分,再采用直观推导式演进特征投影（HELP）法分辨色谱重叠峰,通过质谱库进行定性,采用总体积积分法进行定量。结果：生姜和生姜皮的挥发油分别定性出了51和62个成分,分别占总含量的74.84%和82.55%。结论：生姜与姜皮共...     

水产品中残留氯霉素的分析——NCI源GC／MS分析方法

随着美．日，欧等国对进口食品中的抗生素含量的检测标准一再提高．对于我国的产品出口企业和检测监督部门来说，应用更高灵敏度的分析方法，以适应各国不断提高的新标准．就成为一项十分重要与紧迫的工作。本文介绍的NCI源气相色谱质谱联用检测水产品中氯霉索残留的方法．就具有灵敏度高、回收率和稳定性良好等特点，值得相关领域的读者借鉴。     

"翔安邨"清香型高梁酒主要香气成分的GC/MS分析

采用气相色谱／质谱法对以乙醚提取的“翔安郦”白酒中香气成分进行了分析鉴定,共分离和初步鉴定22个芳香性成分。其中主要芳香性成分是乙酸乙酯、乳酸乙酯、辛酸乙酯、棕榈酸乙酯、异戊醇、异丁醇等。     

PTR—MS与GC／MS在VOCs分析中的比较

挥发性有机物（VOCs）分析通常使用气相色谱／质谱（GC／MS）联用技术,但该技术对VOCs痕量分析仍有待改进。质子传递反应质谱（PTR-MS）技术弥补了GC／MS技术检测VOCs种类受限及耗时、费力等不足,本文通过测试室内低浓度VOCs,对比讨论了两种技术的性能及优缺点。     

高纯惰性气体的气相色谱—质谱联用分析

介绍了高纯稀有气体氮、氖、氩、氪、氙的气相色谱－质谱取用分析技术及实验方法。     

塑料包装材料中邻苯类化合物提取方法的比较

用气相色谱-质谱法(GC-MS)测定了塑料包装材料中邻苯类化合物。比较了正己烷、二氯甲烷等提取溶剂,分别考察索式抽提、超声提取、振荡提取、微波萃取等4种提取方法和提取时间等因素,对提取塑料包装材料中16种邻苯类化合物的影响。选用了正己烷超声提取,气相色谱-质谱法分析,并选择离子扫描(SIM)定量。该方法简便、快捷、准确,适用于各类塑料包装材料中邻苯类化合物的检测。     

菠萝香气成分的GC/MS分析

采用固相微萃取(SPME)方法提取成熟菠萝的芳香物质,经气相色谱-质谱联机(GC/MS)分析,结合计算机检索技术对分离化合物进行鉴定,应用色谱峰面积归一法测定各成分的相对含量。检测结果表明:共鉴定出29种芳香物质成分,约占总峰面积的91.53%,其中分离出烃类(8种,27.6%)、酯类(8种,27.6%)、酮类(3种,10.3%)、醇类(3种,10.3%)、醛类(2种,6.8%),还有酚、呋喃、酸、杂环、胺类各一种各占3.4%。为进一步评价菠萝品质和利用芳香物质提供基础数据。     

气相色谱-质谱测定化妆品中的硝基麝香类化合物

建立了化妆品中5种硝基麝香含量的气相色谱-质谱联用检测方法。采用丙酮/正己烷混合液超声提取化妆品中的硝基麝香,提取液经过浓缩,由气相色谱-质谱联用仪检测,以氘代二甲苯麝香内标法定量。该方法对化妆品中5种硝基麝香的加标回收率在85.21%~110.2%之间,相对标准偏差(RSD)不大于7.15%,在50μg/L~5000μg/L范围内呈现良好的线性关系,灵敏度高,最低检测限分别达到20~50μg/kg;选择性好,能有效消除复杂基体干扰。可用于常见化妆品中硝基麝香类化合物含量的检测。     

分散液液微萃取-气相色谱-质谱分析尿样中的氯氮卓

目的:用分散液液微萃取-气相色谱-质谱联用技术提取检测生物检材中的氯氮卓。方法:以氯仿为微萃取剂,甲醇为分散剂,在pH8提取尿样中的氯氮卓,气相色谱-质谱法分析,用内标标准曲线法测定氯氮卓的含量。结果:尿样中氯氮卓的线性范围为0.01～2μg/ml,检出限为0.002?g/ml;方法回收率为87.3%,RSD=3.47%(n=5)。结论:该方法操作简便、灵敏度高,适于尿样中氯氮卓的快速分析。     

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%。     

气相色谱-质谱联用法测定乳液化妆品中的苯唑卡因

建立了气相色谱-质谱联用仪分析乳液化妆品中苯唑卡因的方法,线性范围0.2~8.0 mg·L-1(r=0.995),方法检测限0.06 mg·L-1(S/N3),1.0 mg·L-1的加标回收率90.7%(n=6)。     

Detection of microbial contamination of packaging for foodstuffs by gas chromatography–mass spectrometry method

Detection of microbial contamination of packaging for foodstuffs and of the environment, using a gas chromatography–mass spectrometry (GC–MS) method, is described. Quantitative determination of muramic acid, a chemical marker of bacterial peptidoglycan, has been used for this purpose. Samples of dust collected from packaging material (plastic film in the store‐room), intended to come into contact with foodstuffs, and dust from a laboratory environment were hydrolysed in aqueous hydrochloric acid and next extracted with hexane to remove hydrophobic compounds. The aqueous phase was evaporated, heated in silylation reagent to trimethylsilyl derivatives and analysed by GC–MS. Internal standard (3‐hydroxytridecanoic methyl ester) was added before silylation procedure for quantification purposes. The method described is quick and simple, can be applied to study chemical markers directly without prior culturing, in complex environmental samples (not only of packaging), and should therefore become widely used for measuring bacterial peptidoglycan. The method can be used for the detection of microbial infection in humans, hospitals, infusing fluids, contamination of biochemical and fermentation processes, and for monitoring of air, water, air‐conditioning systems, etc. Copyright © 2002 John Wiley & Sons, Ltd.     

Thermogravimetry-evolved gas analysis-mass spectrometry system for materials research

Thermal analysis is a widely used analytical technique for materials research. However, thermal analysis with simultaneous evolved gas analysis describes the thermal event more precisely and completely. Among various gas analytical techniques, mass spectrometry has many advantages. Hence, an ultra high vacuum (UHV) compatible mass spectrometry based evolved gas analysis (EGA-MS) system has been developed. This system consists of a measurement chamber housing a mass spectrometer, spinning rotor gauge and vacuum gauges coupled to a high vacuum, high temperature reaction chamber. A commercial thermogravimetric analyser (TGA: TG + DTA) is interfaced to it. Additional mass flow based gas/vapour delivery system and calibration gas inlets have been added to make it a versatile TGA-EGA-MS facility. This system which gives complete information on weight change, heat change, nature and content of evolved gases is being used for (i) temperature programmed decomposition (TPD), (ii) synthesis of nanocrystalline materials, (iii) gas-solid interactions and (iv) analysis of gas mixtures. The TPD of various inorganic oxyanion solids are studied and reaction intermediates/products are analysed off-line. The dynamic operating conditions are found to yield nanocrystalline products in many cases. This paper essentially describes design features involved in coupling the existing EGA-MS system to TGA, associated fluid handling systems, the system calibration procedures and results on temperature programmed decomposition. In addition, synthesis of a few nanocrystalline oxides by vacuum thermal decomposition, gas analysis and potential use of this facility as controlled atmosphere exposure facility for studying gas-solid interactions are also described.     

Assessment of the co-elution problem in gas chromatography-mass spectrometry using non-linear optimization techniques

Multivariate curve resolution based on the minimization of an objective function (MCR-FMIN) defined directly from the non-fulfillment of constraints was applied for the first time as a deconvolution method to separate co-eluted gas chromatographic-mass spectrometric (GC-MS) signals. Simulated and real (standard real mixture and limon oil) GC-MS data were used to evaluate the feasibility of this method. The MCR-FMIN solutions have been obtained based on the rotation of principal component analysis (PCA) solutions using the non-linear optimization algorithms. Calculation of the initial values of R rotation matrix using model free analysis methods such as fixed-size moving window-evolving factor analysis (FSMW-EFA), evolving latent projective graphs (ELPGs), and heuristic evolving latent projection (HELP) was proposed for faster convergence and avoiding to be stuck in local minima in MCR-FMIN algorithm. The band boundaries of feasible solutions (MCR-BANDS) obtained using MCR-FMIN were calculated for simulated data to assess the reliability of the method. In addition, the results of this method were compared with those of two most common self-modeling curve resolution (SMCR) methods of multivariate curve resolution-alternating least square (MCR-ALS) and HELP. A reasonable result can be obtained by selecting proper constraints, such as non-negativity, unimodality, normalization, and selectivity. However, when the number of components or the level of noise in each peak cluster increase, the convergence of algorithm becomes difficult and the results are not reliable. For quick and accurate analysis of co-eluted multi-component problematic GC-MS data MCR-FMIN can be considered as an alternative method to the MCR-ALS and HELP methods.     

气相色谱-质谱法测定卷烟接装纸中的己二酸酯

建立气相色谱-质谱法测定卷烟接装纸中己二酸酯的方法,采用超声辅助异丙醇萃取,DB-5MS色谱柱分离,选择离子检测,内标法定量。己二酸酯在0.05～2.00μg/mL浓度范围内具有良好的线性关系,相关系数大于0.999,加标回收率为78.84%～112.62%,RSD<9%,检出限为0.0051～0.0211mg/kg。证明该方法快速、简便易行,可作为测定卷烟接装纸中己二酸酯的方法。