调味品中氯丙醇的GC/ECD和GC/MS/MS衍生化检测方法研究及应用

报道了调味品中氯丙醇的衍生化气相色谱(GC／ECD)和衍生化气相色谱双串联质谱法(GC／MS／MS)测定。GC／ECD测定酱油中3—氯—1,2—丙二醇(3—MCPD)的检出限达到0．01mg／kg,回收率为91％～104％,变异系数为2．27％～7．96％;GC／MS／MS同时测定酱油中1,3—二氯—2—丙醇、2,3—二氯—1—丙醇和3—氯—1,2—丙二醇,1,3—二氯—2—丙醇、2,3—二氯—1—丙醇的检出限为0．02mg／kg,3—氯—1,2—丙二醇的检出限为0．01mg／kg,回收率在92％～106％,变异系数为3．51％～13．33％。     

烟草制品中紫苏葶的气相色谱/质谱法分析

以二氯甲烷为溶剂,丙酸苯乙酯为内标,将烟草制品进行萃取,经固相萃取柱纯化,采用气相色谱／质谱法定量分析了烟草制品中的紫苏葶．方法的定性检测限为0．11μ/g,定量检测限为0．36μ/g,平均回收率为95．53％,相对标准偏差（RSD）为1．89％．     

Adsorption Kinetics and Dynamic Behavior of a Carbon Monolith

The zero length column (ZLC) method has been applied to study the adsorption and diffusion of CO₂ in a carbon monolith adsorbent. ZLC desorption curves, measured over a wide range of flow rates, are shown to be very well accounted for assuming a linear equilibrium isotherm with the kinetics controlled by diffusion into a parallel sided slab. The data, at all flow rates, are characterized by a single pair of parameters (K and D _s). Diffusivities for a He carrier are about double those for a N₂ carrier reflecting both the difference in molecular diffusivities and some contribution from Knudsen diffusion. Breakthrough curves for CO₂-He and CO₂-N₂ were also measured for columns packed with the monolith adsorbent. Both the equilibrium and diffusion parameters derived from analysis of the breakthrough curves in accordance with the Golay/Spangler models are consistent with the values derived from the ZLC measurements. Dispersion in the monoliths is shown to be controlled by mass transfer resistance rather than axial mixing.     

葡萄酒中白藜芦醇的固相萃取GC/MS法测定及其生理活性的初步研究

用反向C₁₈固相萃取小柱对葡萄酒进行了预处理,然后用BSTFA硅烷化试剂对萃取物进行了衍生化处理,用气相色谱/质谱对葡萄酒中顺式、反式白藜芦醇进行了同时测定,建立了定量分析方法.对方法的精密度和回收率进行了测定,方法的相对标准偏差分别为4.48%(顺式)和5.23%(反式).顺式、反式白藜芦醇的平均回收率分别为94.4%和97.6%.并对10种国产葡萄酒和两种进口葡萄酒样品进行了测定.对白藜芦醇的生理活性也进行了实验,初步探讨了白藜芦醇对大鼠血管平滑肌细胞(VSMC)、大肠癌细胞株Lovo细胞和小鼠成纤维株3T3细胞的生长生殖活性的影响,观察了其形态变化.     

GC／MS法分析鳗鱼骨油的脂肪酸

用乙醚／已烷混合溶剂抽提鳗鱼骨油，用ＫＯＨ－ＣＨ_３ＯＨ酯交换法甲酯化，以毛细管色谱／质谱方法测定脂肪酸的组成。共检出２７种脂肪酸，其中以棕榈油酸、棕榈酸、油酸、硬脂酸、花生烯酸为主。     

GC/MS测定锅巴中丙烯酰胺含量

建立了一种测定市售锅巴中的丙烯酰胺含量的方法.该法样品前处理不必经过溴化衍生,样品脱脂后用水提取丙烯酰胺,提取液过活性炭柱,再用乙酸乙酯将活性炭柱中吸附的丙烯酰胺洗脱.洗脱液浓缩后经气相色谱-质谱(GC-MS)定量分析,检测限为0.06 mg/kg,适合测定市售锅巴中的丙烯酰胺的含量.还考察了丙烯酰胺在水的固液两相中的分配比.     

气相色谱-质谱联用分析2-氯-5-三氯甲基吡啶

2-氯-5-三氯甲基吡啶是重要的农药中间体.采用气相色谱-质谱联用法,对高效除草剂盖草能的中间体2-氯-5-三氯甲基吡啶的分析条件进行了探讨和优化.使用Rts-5MS毛细管柱,EI电离源,实验结果的线性关系良好,相关系数r=0.9921,回收率为99.05%,相对标准偏差为0.78%.     

GC/MS法测定大米中精噁唑禾草灵和氰氟草酯残留量

采用乙腈提取,NH2固相萃取柱净化,GC/MS测定,建立了大米中精噁唑禾草灵和氰氟草酯残留量的测定方法.添加精噁唑禾草灵质量分数为0.02,0.2,0.5mg/kg,平均回收率分别为82.3％,88.8％和90.7％,相对标准偏差分别为6.8％,8.2％和3.7％,检出限为0.02 mg/kg;添加氰氟草酯质量分数为0.02,0.2,0.5mg/kg,平均回收率分别为87.7％,94.2％和92.3％,相对标准偏差分别为8.6％,5.6％和7.3％,检出限为0.02mg/kg.     

Determination of estrogens and progestogens by mass spectrometric techniques (GC/MS, LC/MS and LC/MS/MS)

Steroid sex hormones and related synthetic compounds have been shown to provoke alarming estrogenic effects in aquatic organisms, such as feminization, at very low concentrations (ng/L or pg/L). In this work, different chromatographic techniques, namely, gas chromatography/mass spectrometry (GC/MS), liquid chromatography/mass spectrometry (LC/MS) and liquid chromatography/tandem mass spectrometry (LC/MS/MS), are discussed for the analysis of estrogens, both free and conjugated, and progestogens, and the sensitivities achieved with the various techniques are inter-compared. GC/MS analyses are usually carried out after derivatization of the analytes with bis(trimethylsilyl)trifluoroacetamide (BSTFA). For LC/MS and LC/MS/MS analyses, different instruments, ionization techniques (electrospray (ESI) and atmospheric pressure chemical ionization (APCI)), ionization modes (negative ion (NI) and positive ion (PI)) and monitoring modes (selected ion monitoring (SIM) and selected reaction monitoring (SRM)) are generally employed. Based on sensitivity and selectivity, LC/ESI-MS/MS is generally the method of choice for determination of estrogens in the NI mode and of progestogens in the PI mode (instrumental detection limits (IDLs) 0.1-10 ng/mL). IDLs achieved by LC/ESI-MS in the SIM mode and by LC/ESI-MS/MS in the SRM mode were, in general, comparable, although the selectivity of the latter is significantly higher and essential to avoid false positive determinations in the analysis of real samples. Conclusions and future perspectives are outlined.     

林蛙油中农药残留的GC-MS/MS检测方法

首次建立了林蛙油中15种农药（p,p′DDE,O,p′-DDD,o p′-DDT,p,p′-DDT,BHC（α、β、γ、δ）,异丙威,甲拌磷,六氯苯,百菌清,皮蝇磷,倍硫磷,甲氰菊酯）的GC—MS／MS残留检测方法。样品用乙酸乙酯提取、Florisil层析柱净化后,经GC—MS／MS检测,用外标法定量。15种农药在0．050～10．0mg／L范围内,线性关系良好,相关系数r≥0．996。当添加量在0．050—2．00mg／kg间,平均加标回收率为81％～117％,RSD为2．4％-18．2％,方法的检出限为0．050mg／kg。该方法准确、灵敏,适用于农药残留的分析。     

Determination of wine aroma compounds by dehydration followed by GC/MS

A new extraction method for the analysis of the volatile fraction of white and red wines has been developed and validated. A dehydration step with MgSO4 separated an aroma compounds-rich alcoholic-glycerine layer. Spiked samples showed good recoveries in the range between 75 and 120% with CVmax% of 17, except for 2-phenylethanol and y-butyrolactone for which recoveries in red wines were under 60%, and for monoethylsuccinate, where recoveries averaged 50 and 60% in white and red wines, respectively. Method repeatability and intermediate precision showed good CVmax% with minimum and maximum values between 7.7 and 24, and between 18.7 and 25.0, respectively. The average determination coefficients were greater than 0.99 with CVmax% of 13. The instrumental LOD and LOQ were, in all cases, under 0.05 mg/L, except for 2,3 butanediol (0.20 mg/L). Overall, the presence of wine matrix affected aroma compounds responses in GC/MS analysis. These observations indicate that the use of a matrix-matched calibration curve is mandatory to obtain reliable quantitative data.     

Determination of N-n-alkyl-dimethylmorpholines and their metabolites by high resolution GC/MS

An analytical method is described to determine simultaneously cis/trans N-n-alkyl-dimethylmorpholines and their metabolites, the 4-(ω-carboxy-n-alkyl) cis/trans-2,6-dimethylmorpholines by pyrolytic alkylation and high resolution GC/MS in aqueous systems and sediments. The substances in the sediment phase were analyzed by GC/MS after extraction with methanol and water, substances in the water phase could be directly determined by GC/MS. The analytical procedure also allows the determination of further carboxylic acids in complex aqueous systems. Received: 9 April 1996 / Revised: 10 June 1996 / Accepted: 14 June 1996     

气相色谱-质谱测定保健食品中的麻黄碱和伪麻黄碱

麻黄为麻黄科植物,是一种传统中药,含苯烃基胺类生物碱,主要为麻黄碱、伪麻黄碱和微量l-N-甲基麻黄碱、d-N-甲基伪麻黄碱、d-去甲伪麻黄碱等,用于治疗风寒感冒、胸闷喘咳、风水浮肿、支气管哮喘^[1]。同时它也有毒副作用,国际奥委会把它列为禁用药品,许多国家禁止其在食品、保健品中使用。测定麻黄碱的方法已有很多^[2-5],但具有各自     

棕榈油中脂肪酸的GC/MS定性分析

本文介绍了进口棕榈油中的脂肪酸的色-质联用分析方法。其中,特别检测了油中的奇碳数脂肪酸,并和其它食用油中的脂肪酸作了比较。     

Determination of Aroma Compounds in Blackberry by GC/MS Analysis

The aromatic composition of five blackberry cultivars (Bursa 2, Navaho, Nessy, Chester Thornless, and Jumbo) was studied. The Im-SPME (Immersion Solid Phase Micro Extraction) extraction technique was applied and the samples were analyzed by GC/MS. Furfural and its derivatives were found to be the major aromatic compounds and 5-hydroxymethylfurfural was the most abundant compound in all the blackberry varieties.     

Determination of N-n-alkyl-dimethylmorpholines and their metabolites by high resolution GC/MS

An analytical method is described to determine simultaneously cis/trans N-n-alkyl-dimethylmorpholines and their metabolites, the 4-(ω-carboxy-n-alkyl) cis/trans-2,6-dimethylmorpholines by pyrolytic alkylation and high resolution GC/MS in aqueous systems and sediments. The substances in the sediment phase were analyzed by GC/MS after extraction with methanol and water, substances in the water phase could be directly determined by GC/MS. The analytical procedure also allows the determination of further carboxylic acids in complex aqueous systems.     

夏蜡梅挥发油气相色谱-质谱研究

引　　言夏蜡梅 (calycanthuschinensis) ,又称牡丹木、黄枇杷、大叶棠 ,为蜡梅科 (calycanthaceae) ,夏蜡梅属 (calycanthusL .)。在原产地浙江临安为落叶灌木。它为我国特有的第三纪孑遗植物 ,具有重要的植物系统学研究价值及药用、观赏价值。夏蜡梅叶对感冒、咳嗽、气喘等具有一定的疗效。文献检索发现 ,除了少量有关蜡梅科植物的挥发组分的零星报道外 ,至今未有关夏蜡梅挥发油成分的详细报道。本文首次较详细、深入地报道了夏蜡梅成熟叶的挥发性化学成分 ,旨在为生药鉴定、深入开发利用及种质资源的有效保护提供科学依据。2　实验部…     

气相色谱-质谱法测定卷烟烟气总粒相物中的乳酸

以三甲基氢氧化硫为甲酯化试剂,正戊醇为内标,采用CP-FFAP毛细管柱(25 m×0.15 mm i.d.×0.25μm d.f)和选择离子模式,建立了卷烟烟气总粒相物中乳酸的气相色谱-质谱分析方法。该方法的线性范围为0.285~0.0570mg/mL乳酸(r=0.9997),平均回收率为97.99%,RSD为1.58%。并用该法测定了部分卷烟烟气总粒相物中的乳酸。     

Determination of Inhalational Anesthetics in Field and Laboratory by SPME GC/MS

Exposure to inhalational anesthetics in health care workers could lead to several diseases and disorders. This study examined the applicability of solid phase microextraction for sampling and quantification of three inhalational anesthetics including; halothane, isoflurane, and sevoflurane in operating room air. Carboxen-Polydimethylsiloxane in retracted mode was selected and the effects of environmental parameters including temperature, humidity, and air velocity, were studied. There were no significant differences between sampling rates determined at different temperatures and air velocities. On the opposite, relative humidity has a significant effect on sampling rates. Comparison of the results between the developed SPME method and OSHA 103 method on standard test atmosphere and field showed satisfactory agreement.     

Determination of different recreational drugs in hair by HS-SPME and GC/MS

A simple procedure combining headspace solid-phase microextraction (HS-SPME) and gas chromatography–mass spectrometry (GC/MS) to detect and quantify amphetamines, ketamine, methadone, cocaine, cocaethylene and ∆⁹-tetrahydrocannabinol (THC) in hair is described. This procedure allows, in a single sample, even scant, analysis of drugs requiring different analytical conditions. A hair sample (10 mg) is washed and subjected to acidic hydrolysis. Then the HS-SPME is carried out (10 min at 90 °C) for amphetamines, ketamine, methadone, cocaine and cocaethylene. For derivatization of analytes, the fibre is introduced into the headspace of another closed vial containing acetic anhydride. After a chromatographic run, an alkaline hydrolysis for THC analysis is carried out in the same vial containing the hair sample previously used. For adsorption, the solid-phase microextraction needle is inserted into the headspace of the vial and the fibre is exposed for 30 min at 150 °C. For derivatization of analytes, the fibre is introduced into the headspace of another closed vial containing N-methyl-N-(trimethylsilyl)trifluoroacetamide. The GC/MS parameters were the same for both chromatographic runs. The linearity was proved to be between 0.01 and 10.00 ng/mg. The repeatability (intra- and interday precision) was below 10% as the coefficient of variation for all compounds. The accuracy, as the relative recovery, was 96.2–103.5% (spiked samples) and 88.6–101.7% (quality control sample). The limit of detection ranged from 0.01 to 0.12 ng/mg, and the limit of quantification ranged from 0.02 to 0.37 ng/mg. Application of the procedure to real hair samples is described. To the best of our knowledge, the proposed procedure combining HS-SPME and GC/MS is the first one be to successfully applied to the simultaneous determination of most of the common recreational drugs, including THC, in a single hair sample.