全自动固相微萃取-气相色谱联用测定土壤中的多氯联苯

建立了简单可靠的自动固相微萃取-气相色谱联用测定土壤中的六种指示性多氯联苯(PCBs).同时研究了主要环境因素对方法萃取效率的影响.结果表明对六种分析物来说,用100μm的PDMS萃取头,在100℃的条件下萃取40 min能够得到较好的萃取效果.该方法简便、快捷、成本低,线性良好,检测限低至0.1～0.2 ng·g1,...     

固相微萃取-气相色谱法测定食品添加剂中有害有机挥发杂质

建立了固相微萃取（SPME）-气相色谱法（GC）测定食品添加剂中有害有机挥发杂质：二氯甲烷、三氯甲烷、苯、三氯乙烯和1、4-二n恶烷的方法。以聚二甲基硅氧烷（PDMS）涂层的萃取纤维萃取糖精钠、柠檬酸、苯甲酸钠溶液中的待测组分。以HP-5毛细管柱为分离柱，火焰离子化检测器（FID）定量测定。优化了固相微萃取条件：萃取纤维、萃取方式、萃取温度、平衡时间、pH及电解质浓度等。在优化的试验条件下，进行了方法的检出限、精密度、回收率试验。5种组分的回收率在97．3％～103．9％之间。     

固相微萃取-气相色谱联用技术分析饮用水中的氯仿

利用顶空固相微萃取与气相色谱联用技术（ＨＳ－ＳＰＭＥ－ＧＣ）对饮用水中的氯仿进行了分析,并探讨了ＳＰＭＥ萃取头、吸附和热解吸时间对测定结果的影响;聚丙烯酸酯（ＰＡ）萃取头对水中的氯仿有较佳的富集效果,方法具有较好的重现性（ＲＳＤ为５．２３％,ｎ＝８）,线性范围为５～１００μｇ／Ｌ,检出限为３．４５μｇ／Ｌ。     

固相微萃取-气相色谱-质谱联用测定水中酚类化合物

建立了固相微萃取与气相色谱－质谱联用技术（SPME－GC－MS）测定水中酚类化合物的新方法，探讨了萃取时间、搅拌速度、离子强度、pH值和解吸时间等条件对萃取量的影响。结果表明：65μm PDMS/DVB涂层对水中的酚类化合物有较好的萃取效果，用于水中酚类化合物的测定，结果满意。     

固相微萃取-气相色谱法测定塑料食品包装袋中的痕量挥发性有机物

采用固相微萃取与气相色谱联用技术，对塑料制品-保鲜薄膜、牛奶包装袋中的痕量挥发性有机物异丙醇、乙酸乙酯、丁酮、甲苯进行定量测定．该方法的线性范围大于l0^2数量级，检出限低于4．4ng/mL水平，相对标准偏差为2.3％-4．7％．方法灵敏度高、重现性较好．     

活性炭固相微萃取-气相色谱联用测定海水中酞酸酯

利用自制的活性炭纤维结合固相微萃取-气相色谱联用技术(ACF-SPME-GC)分析了海水中4种邻苯二甲酸酯.对萃取温度、离子强度、吸附和热解吸时间等影响因素进行了研究.结果表明,在盐浓度为15%和萃取温度为60 ℃条件下萃取60 min,效果最好.在最优化条件下,本方法的线性范围为0.1～1000 μg/L; 检出限为0.01～10 μg/L; 相对标准偏差均小于10%.将ACF-SPME-GC技术用于实际海水样品的分析,未检测出这4种邻苯二甲酸酯化合物.     

固相微萃取/气相色谱-质谱联用技术测定燕窝中挥发性成分

该文以印尼产的燕窝为材料,使用固相微萃取(SPME)技术萃取燕窝中挥发性成分并以气相色谱-质谱(GC-MS)联用仪进行测定。考察了萃取头类型、萃取温度、萃取时间和解吸时间对固相微萃取(SPME)在燕窝挥发性成分测定中的影响。结果表明:以65μm聚二甲基硅氧烷/二乙烯基苯(PDMS/DVB)萃取头、在60℃下萃取60 min,解吸2 min的条件下,SPME/GC-MS技术可检出燕窝中挥发性成分醇、烃、醛、酯、醚类等化合物共82种。该方法具有操作简便、快速、重复性好和灵敏度高的特点,适用于燕窝中挥发性成分的测定。     

固相微萃取-气相色谱-质谱法测定饮用水源中53种挥发性有机污染物

应用固相微萃取-气相色谱-质谱法测定饮用水源中53种挥发性有机污染物的含量。优化的试验条件如下:1萃取纤维为DVB/CAR/PDMS;2萃取温度为25℃;3顶空体积为9mL;4萃取时间为10min;5解吸温度为200℃;6解吸时间为3min。在气相色谱分离中用VF-624MS柱为固定相,在质谱分析中采用全扫描模式。53种挥发性有机污染物在一定的质量浓度范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.001~0.130μg·L-1之间。方法用于实际水样的分析,加标回收率在75.9%~107%之间,测定值的相对标准偏差(n=5)在0.5%~18%之间。     

顶空固相微萃取-气相色谱法测定废水中挥发性脂肪酸

提出了顶空固相微萃取-气相色谱法测定废水中挥发性脂肪酸(乙酸、丙酸、丁酸、戊酸、异戊酸和己酸)的含量。为使固相微萃取达到更高的效率,选择极性85μm PA作为微萃取头的涂层,微萃取系在pH 1.5的试液中进行,萃取温度及时间为25℃和20 min,在20 mL试样溶液中加入氯化钠3.5 g作为盐析剂。用Stabilwax-DA毛细管色谱柱分离,火焰离子检测器检测。6种脂肪酸在一定的质量浓度范围内与其峰面积呈线性关系,相对标准偏差(n=10)均小于10.0%。     

固相微萃取-气相色谱-质谱技术分析槐花的挥发性成分

用顶空固相微萃取操作,结合气相色谱-质谱联用技术对槐花挥发性成分进行了鉴定,并用面积归一化法测定其相对含量.共鉴定出化合物31种,包括酮、醇、酸、甾醇、酚、醛、酯、烷烃、烯烃及杂环等10类化合物,其中酮类化合物占总色谱馏出峰面积的21.15%;醇类化合物占13.78%;酸类占9.15%.其主要化合物有:1,9,12三氧-4,6-二氨基环十四烷-5-硫酮(20.58%),棕榈酸(9.05%),9,12,15-十八三烯醇(7.05%),(Z,Z)-9,12-十八碳二烯酸(6.85%),β-谷甾醇(6.11%).该技术可以简便快捷准确地进行槐花挥发性成分的分析鉴定.     

Determination of volatile fatty acid ethyl esters in raw spirits using solid phase microextraction and gas chromatography

An analytical method for the determination of fatty acid ethyl esters in raw spirits of different quality or produced from various raw materials has been developed and optimized. A combination of headspace solid phase microextraction (HS-SPME) as the extraction technique and gas chromatography with flame ionization detection (GC-FID) as the determination technique was utilized. HS-SPME conditions such as: type of the stationary phase of the fiber, ethanol content, sample volume, extraction temperature and time, salt addition and sample agitation were investigated to determine the most suitable conditions for the analysis of volatile fatty acid ethyl esters in raw spirits. The quantification method was an internal standardization using methyl octanoate as the internal standard. The method's detection limits (MDLs) for the individual ethyl esters ranged from 26.8 to 0.0470 μg L⁻¹ 20% EtOH. The feasibility of SPME for the quantitative analysis of fatty acid ethyl esters in raw spirits of different organoleptic quality was demonstrated. High precision and simple sample preparation enable the use of this method for routine investigations in both industrial and research laboratories.     

SPME-GC联用测定环境水样中的酚类化合物

建立了固相微萃取与气相色谱联用技术测定环境水样中酚类化合物的方法. 探讨了pH、离子强度、萃取头类型、萃取时间以及解析时间等条件对酚类化合物萃取量的影响, 优化了GC仪器条件. 在优化的条件下, 酚类化合物的响应值与浓度有良好的线性关系, 线性范围为0.20～200 μg/L, 检出限在0.019～0.10 μg/L之间, 相对标准偏差(RSD, n=5)为4.4%～11%, 水样平均加标回收率为92.2%～101.9%, 所建立的方法可测定环境水样中的酚类化合物.     

Determination of organic acid impurities in lactic acid obtained by fermentation of sugarcane juice

Lactic acid produced by fermentation process mostly contains a number of aliphatic carboxylic acids as impurities. In this work, carboxylic acid impurities in lactic acid samples from a number of sources were determined at ppm levels. A simple HPLC method was developed that utilized a new generation polar embedded reverse phase, 20mM phosphate buffer at pH 2.20 (±0.05) and UV detection at 210 nm. The method enabled quantitative analysis of the above acids in lactic acid matrix. The experimental conditions for column temperature, mobile phase pH and flow rate were optimized. A detailed validation of the method was performed for linearity, precision, accuracy, selectivity, limit of detection (LOD), limit of quantitation (LOQ), ruggedness and repeatability and reproducibility (R&R).     

固相微萃取-气相色谱联用技术测定水相中的邻苯二甲酸二(2-乙基)己酯

利用顶空固相微萃取与气相色谱联用技术（HS－SPME－GC）以富勒烯聚二甲基硅氧烷（PSO－C60）固定相处制萃取头分析了塑料浸取液中的邻苯二甲酸二（2－乙基）己酯（DEHP），并对萃取温度、离子强度、吸附时间和热解析时间进行了研究。结果显示，该方法的线性范围在5μg/L－500μg/L，检测出了为2．8μg/L，相对标准偏差为4．8％（n=6).     

柠檬酸试剂中痕量无机阴阳离子的离子色谱法测定

选用柱容量较高、亲水性较强的阴离子分析柱IonPac AS18,以30mmol／L KOH为淋洗液,等度淋洗分析了高浓度柠檬酸中的痕量无机阴离子。选用柱容量较高的阳离子分析柱IonPac CS12A,以H2SO4作淋洗液分析了柠檬酸试剂中的痕量阳离子。在所选色谱条件下,无需样品前处理,直接进样,电导检测,高浓度柠檬酸不影响痕量阴离子或阳离子的测定。方法具有良好的线性(r=0．9941～1．000),样品中所测离子峰面积的相对标准偏差(RSD)均在9．0％以下(n=7),回收率在82．7％～110％之间,检出限低于3．7μg/L。     

Preconcentration of poorly volatile impurities in thin-layer chromatography by thermodesorption of a volatile matrix

A method for preconcentration of poorly volatile impurities by continuous thermodesorption of the major component on a TLC plate is proposed. The method provides multiple (200–500) concentration of the organic impurities present in the initial solution. A simple device for such concentration is suggested. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 10, pp. 2075–2076, October, 1998.     

Determination of volatile aliphatic amines in air by solid-phase microextraction coupled with gas chromatography with flame ionization detection

Practical aspects of the application of solid-phase microextraction (SPME) to the determination of volatile aliphatic amines in air are described. Analytes included methylamine (MA), ethylamine (EA), dimethylamine (DMA), diethylamine (DEA), trimethylamine (TMA) and triethylamine (TEA). New SPME stationary phases were examined. The effects of relative humidity and temperature on analytes uptake were taken into account in analysis. Gas chromatography (GC) with flame ionization detector (FID) was used for the final analysis.     

顶空固相微萃取-气相色谱-质谱联用分析纺织品中挥发性有机物

建立了顶空固相微萃取（HSSPME）-气相色谱（GC）-质谱（MS）联用测定纺织品中甲苯、4-乙烯基环己烯、苯乙烯、萘和1-苯基环己烯5种挥发性有机物（VOCs）的分析方法。选择聚二甲基硅氧烷（PDMS）作为萃取涂层,优化了SPME的萃取条件,包括平衡时间、萃取时间、萃取温度、顶空体积、离子强度、搅拌速度、解吸温度和时间以及GC—MS仪器条件。对于甲苯、4-乙烯基环己烯、苯乙烯、萘和1-苯基环己烯方法线性范围分别为0．087～870、3．32～3320、2．28～2280、0．015～150和0．050～50．0ng／g;检出限分别为0．005、0．042、0．670、0．008和0．011ng／g。实际样品加标回收率在80．1％～122％之间,RSD在0．8％～8．6％之间。方法符合纺织品中痕量VOCs的快速分析要求。     

Determination of volatile organic compounds in the dried leaves of Salvia species by solid-phase microextraction coupled to gas chromatography mass spectrometry

Salvia spp. are used throughout the world both for food and pharmaceutical purposes. In this study, a method involving headspace solid-phase microextraction combined with gas chromatography–mass spectrometry was developed, to establish the volatiles profile of dried leaves of four Iranian Salvia spp.: Salvia officinalis L., Salvia leriifolia Benth, Salvia macrosiphon Boiss. and two ecotypes of Salvia reuterana Boiss. A total of 95 volatiles were identified from the dried leaves of the five selected samples. Specifically, α-thujone was the main component of S. officinalis L. and S. macrosiphon Boiss. (34.40 and 17.84%, respectively) dried leaves, S. leriifolia Benth was dominated by β-pinene (27.03%), whereas α-terpinene was the major constituent of the two ecotypes of S. reuterana Boiss. (21.67 and 13.84%, respectively). These results suggested that the proposed method can be considered as a reliable technique for isolating volatiles from aromatic plants, and for plant differentiation based on the volatile metabolomic profile.