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固相萃取/气相色谱-质谱联用法分析地表水中的半挥发性有机物 总被引:1,自引:0,他引:1
采用固相萃取/气相色谱-质谱联用法分析地表水中的52种半挥发性有机物,方法检出限在0.04-0.13μg/L之间,各化合物回收率均处于EPA 8270及EPA 525所提供的参考范围之内。 相似文献
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利用固相萃取/气相色谱质谱联用技术(SPE/GC-MS),建立了水中33种半挥发性有机物(SVOCs)的高灵敏度检测方法。方法对5~300ng/L SVOCs的线性关系良好(r2>0.99),且定量限(S/N=10)均小于1 ng/L。在10、50、200 ng/L的加标水平下,目标化合物的加标回收率为60.2~116.6%,相对标准偏差为1.69%~15.92%(n≥5)。这说明该方法对水源水中痕量的SVOCs富集效果较好,检测灵敏度高。运用该方法对杭州市不同水源水进行定量分析,发现有16种SVOCs至少在一个水源中多次被检出,其中多环芳烃,钛酸酯,多氯联苯均为"优先控制污染物"。 相似文献
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研究固相萃取/气相质谱法测定水中17种半挥发性有机物的定性定量分析方法。应用DB-5MS色谱柱分离定性,30min内17种目标物分离效果好(除p,p’-DDD和o,p-DDT),SIM扫描提取目标化合物定量离子。内标法定量,标准曲线相关系数R20.990,相对标准偏差5%;样品加标回收率在66.2%~136.6%,方法检出限0.01μg/L~0.066μg/L。方法的灵敏度、精密度和回收率均能满足地表水,饮用水和地下水等17种挥发性有机物痕量分析的要求。 相似文献
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用固相微萃取(SPME)、同时蒸馏萃取(SDE)和液液萃取(LLE)三种前处理方法提取秘鲁浸膏中的挥发性成分,并采用GC-MS法对挥发性成分进行了定性及半定量分析,对这三种萃取方法提取鉴定出的化学成分进行了比较。结果表明:①秘鲁浸膏中主要成分为苯甲酸苄醋,三种萃取方法下的相对质量分数分别为54.90%(SPME)、29.48%(SDE)和67.18%(LLE);②同时蒸馏萃取法提取秘鲁浸膏挥发性成分的鉴定结果中未检测出固相微萃取和液液萃取法中出现的香兰素、乙基香兰素和肉桂酸;③固相微萃取方法简便、快捷、高效,比同时蒸馏萃取、液液萃取更适合于对秘鲁浸膏的提取。 相似文献
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《广州化工》2020,(1)
以二乙烯苯-碳分子-聚二甲基硅氧烷为固相微萃取的吸附涂层进行萃取分离,用气相色谱-质谱联用仪进行测定,建立顶空固相微萃取与气相色谱-质谱联用测定食品中挥发性有机硒(二甲基硒(DMSe)和二甲基二硒(DMDSe))的方法。在最佳测试条件下,DMSe和DMDSe在0.20~900μg/kg和0.05~800μg/kg范围内线性关系良好,拟合系数0.9996和0.9993,检出限分别为0.0570μg/kg和0.0132μg/kg,相对标准偏差(RSDs,n=7)为8.5%和7.1%。方法具有绿色环保、操作简易、灵敏度高等优点,适用于食品中挥发性有机硒的测定。 相似文献
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根据固相微萃取原理,对萃取条件进行了优化。优化后的HS-SPME-GC-MS(顶空固相微萃取/气相/质谱)实验条件为:采用85μm PAA纤维萃取头,萃取时间30min,萃取温度室温,解吸时间5min。在此条件下对3种有机硅乳液进行分析,通过计算机数据系统(质谱数据库NIST和Willy)检索及人工谱图解析,鉴定了非硅油挥发性成分。该方法的相对标准偏差为0·57%~2·59%。 相似文献
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为分析树苔及其提取物中的挥发性及半挥发性化学成分,通过单因素实验优化固相微萃取的萃取头、萃取温度、萃取时间和解吸时间,建立了一种测定树苔及其提取物中挥发性及半挥发性化学成分的顶空-固相微萃取-气质联用法(HS-SPME-GC-MS/MS),并用该方法分析了3种树苔提取物及2种树苔原料。结果表明:优化得到的固相微萃取条件为:0.5 g样品,65μm聚二甲基硅氧烷/二乙烯基苯粉色萃取头,萃取温度90℃,萃取时间20 min,解吸时间2 min; 5种树苔样品中共鉴定出338种(13类)挥发性及半挥发性化学成分,共检出成分有7种,3种树苔提取物主要共有特征成分为苔色酸乙酯、苔黑酚酸甲酯、赤星衣酸甲酯,2种树苔原料主要共有特征成分为苔黑酚酸甲酯。该方法前处理简便快捷、无溶剂损耗,适用于树苔样品的快速定性及半定量分析。 相似文献
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Colin S Creaser David Gmez Lamarca Luisa M Freitas dos Santos Giuseppe LoBiundo Anthony P New 《Journal of chemical technology and biotechnology (Oxford, Oxfordshire : 1986)》2003,78(11):1193-1200
Membrane inlet mass spectrometry (MIMS) has been developed for the on‐line monitoring of compounds in a continuous stirred tank bioreactor (CSTB) used to simulate a wastewater treatment plant (WWTP). A mixture of four industrially relevant nitrogen‐containing volatile and semi‐volatile compounds was fed to a 3 dm3 CSTB with a hydraulic retention time (HRT) of 24 h. In‐membrane preconcentration/thermal desorption was used for the on‐line monitoring of semi‐volatile compounds (n‐methylpyrrolidinone and tetramethylethylenediamine), while volatile organic compounds (3‐bromopyridine and 2‐chloro‐5‐trifluoromethylaniline) were determined by continuous infusion through the membrane. Quantification of the four compounds was achieved by MS. The CSTB was run for 160 h and, after reaching steady state, n‐methylpyrrolidinone showed removal to levels below the limit of detection, while there was partial biodegradation of 2‐chloro‐5‐trifluoromethylaniline and 3‐bromopyridine. There was no evidence of significant biodegradation for tetramethylethylenediamine. Intermediates in the metabolite pathways of 2‐chloro‐5‐trifluoromethylaniline and 3‐bromopyridine were identified by MIMS, gas chromatography/mass spectrometry (GC/MS) or liquid chromatography/mass spectrometry (LC/MS). COD was measured off line, and results agreed well with MIMS, although COD data did not provide information on the removal of the individual compounds. Copyright © 2003 Society of Chemical Industry 相似文献
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马尼拉草是城市草坪中应用最广泛的一种。本实验利用水蒸气蒸馏法研究不同单因素,如浸泡时间、加水量及加热时间对马尼拉草得油率的影响,并做正交试验得出最佳提取条件。同时将最佳提取条件进行优化,采用同时蒸馏萃取法提取,利用气相色谱一质谱联用技术分析马尼拉草挥发油中的化学成分。结果表明,影响马尼拉草挥发油提取效果的最主要因素是加热时间,加水量的影响次之,浸泡时间的影响最小,当浸泡时间为90min、加水量为300mL、加热时间为5h时马尼拉草挥发油的提取效率最大为0.54%;分析可知马尼拉草挥发油中鉴定出24种化合物,包括烯烃、醛类、醇类、醚类、烷烃及酯类。 相似文献
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We evaluated the volatile organic compounds (VOCs) present in human odor by using headspace solid phase microextraction gas chromatography–mass spectrometry for the extraction, separation, and analysis of the collected samples. Volatile organic compounds present in the headspace above axillary sweat samples collected from different individuals showed the presence of various types of compounds including organic fatty acids, ketones, aldehydes, esters, and alcohols. Qualitative differences and similarities noted between the males and females studied along with differences in chemical ratio patterns among the common compounds demonstrated the ability to differentiate between individuals through the examination of VOCs. 相似文献
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采用熔融共混法制备聚丙烯(PP)/滑石粉共混物,利用力学性能测试和热脱附-气相/质谱(TDS-GC/MS)分析手段考察了滑石粉、吸附剂和萃取剂对PP/滑石粉共混物力学性能、熔体流动速率、气味和挥发性有机物(VOC)挥发量的影响。实验结果表明,随着滑石粉、吸附剂和萃取剂含量的增加,PP/滑石粉共混物的气味和总挥发性有机物(TVOC)降低;而吸附剂和萃取剂含量对力学性能几乎没有影响,对熔体流动速率略有影响;另外,随着吸附剂含量的增加,PP/滑石粉共混物的吸湿性会增大,当吸附剂质量分数达到5%时,放置480 h后,其吸水量提高2.7倍;在滑石粉质量分数为20%的PP/滑石粉共混物中,当吸附剂和萃取剂质量分数分别为0.5%,1.0%时,共混物的气味强度和舒适度可分别达到2.5级和0级,TVOC挥发量较挤出后的纯PP下降51%。 相似文献
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A high-volatile bituminous coal was extracted at room temperature by various organic solvents. The yields of the extracts ranged from 4.5 wt% daf (ethanol/benzene extract) to 38 wt% daf (pyridine/ethylenediamine extract). The extracts were analysed by Fl mass spectrometry; the volatile part (75–80 wt%) was composed of substances of molecular weight in the range 70–800 amu, but the compounds in the 200–600 amu range predominated. Over 300 compounds were identified by high-resolution mass spectrometry. The results indicate that compounds < 800 amu constitute at least 30 wt% daf of the analysed coal. 相似文献