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顶空气相色谱法测定化妆品中15种挥发性有机溶剂残留 总被引:1,自引:0,他引:1
建立了化妆品中15种挥发性有机溶剂残留的顶空气相色谱测定方法。样品经60 ℃、30 min静态顶空后,采用气相色谱-氢火焰离子化检测器进行检测,外标法定量。加标回收试验结果表明: 15种挥发性有机溶剂残留平均回收率为62.8%~116%,相对标准偏差均小于5%。方法的检出限为0.09~0.68 mg/kg。该方法可有效克服基体干扰,一次进样可同时分离和测定化妆品中15种挥发性有机溶剂,准确灵敏,简单快速,适用于化妆品中挥发性有机溶剂残留的检测。 相似文献
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以2015版《化妆品安全技术规范》中规定的常见禁用及限用有毒挥发性有机溶剂为研究对象,建立了静态顶空/气相色谱-质谱法(SHS/GC-MS)同时测定化妆品中22种有毒挥发性有机溶剂(VOC)(二氯甲烷、顺式-1,2-二氯乙烯、反式-1,2-二氯乙烯、2-氯-1,3-丁二烯、三氯甲烷、1,2-二氯乙烷、苯、四氯化碳、三氯乙烯、甲苯、四氯乙烯、氯苯、乙苯、三溴甲烷、间二甲苯、对二甲苯、苯乙烯、邻二甲苯、异丙苯、1,4-二氯苯、1,2-二氯苯、六氯丁二烯)残留的检测方法。试样在80℃下30 min静态顶空,经DB-1柱分离后,采用选择离子监测模式(SIM)进行定性定量分析。优化了顶空、色谱和质谱参数,结果表明:22种VOC在0.5~50 ng/m L浓度范围内均呈良好的线性关系,相关系数均大于0.99,在1.0,2.0,5.0 ng/m L 3个浓度加标水平下的平均回收率为80.3%~102.7%,相对标准偏差(RSD,n=6)为6.4%~9.9%,检出限为0.2~5.0 ng/g。结果表明,该方法简便、灵敏、准确,具有良好的重现性和稳定性,适合于化妆品中22种VOC残留的筛查和确证检测。 相似文献
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顶空气相色谱-质谱法测定玩具中的10种挥发性有机物 总被引:1,自引:0,他引:1
建立了检测玩具中10种挥发性有机物(VOC)残留量的顶空气相色谱-质谱(HS-GC-MS)方法。样品经140 ℃、45 min静态顶空后,通过DB-624色谱柱分离和质谱检测,外标法定量。该方法对于不同VOC的定量限(LOQ)均在0.66 mg/kg以下,线性范围为0.001~2.0 μg,平均回收率在79%~106%之间,相对标准偏差(RSD)在0.4%~5.6%之间。该方法具有准确灵敏、简单快速等特点,将其应用于实际玩具样品的检测取得了良好效果。 相似文献
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顶空气相色谱-质谱联用技术的应用进展 总被引:1,自引:0,他引:1
顶空分析作为一种无有机溶剂萃取的样品处理技术,通常与气相色谱-质谱(GC-MS)技术结合用来分析复杂基质中的挥发性有机物。顶空气相色谱-质谱(HS-GC-MS)技术具有快速、高效、环保、灵敏度高等特点,在常规分析中发挥着重要作用。该文简要概述了静态顶空、动态顶空、顶空固相微萃取分析以及GC-MS联用技术,并介绍了整个顶空分析系统的影响因素和优化过程。根据基质类型的分类,综述了HS-GC-MS在食品和饮料、环境、生物等样品中的应用实例。HS-GC-MS的研究非常活跃,不断出现新应用,在分析挥发性有机物方面具有广阔前景。 相似文献
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采用顶空毛细管柱GC–MS法测定饮用水中卤代烃、苯系物、氯苯等15种挥发性有机物。色谱柱为DB–624石英毛细管柱(60 m×0.25 mm,1.8μm),程序升温,直接进样顶空毛细管柱气质联用法同时测定饮用水中15种挥发性有机物。该方法具有良好的线性,线性相关系数均大于0.996。方法的检出限为0.10~0.22μg/L。15种挥发性有机物的平均回收率在94%~103%之间,测定结果的相对标准差为2.9%~6.7%(n=7)。该方法简便、快速,检测结果均能满足GB 5749–2006检测要求。 相似文献
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顶空气相色谱-质谱法同时测定蜂蜜中57种挥发性有机溶剂残留 总被引:1,自引:0,他引:1
建立了顶空气相色谱-质谱(HS-GC/MS)同时测定蜂蜜中57种挥发性有机溶剂(包括烷烃类、芳香烃类、醇类、酮类、酯类、醚类)残留量的分析方法。蜂蜜样品在密封的顶空瓶中用水溶解后,在顶空仪中于80 ℃下平衡30 min,使气-液两相达到动态平衡。采用DB-624毛细管色谱柱(60 m×0.25 mm×1.40 μm)对57种有机溶剂进行分离,GC/MS测定,外标法定量。该方法对于烷烃类、芳香烃类和醚类挥发性有机溶剂在0.005~0.2 μg、酯类0.05~2.0 μg、酮类0.5~20 μg、醇类2.5~100 μg范围内线性关系良好,相关系数均大于0.996。对于烷烃类、芳香烃类和醚类挥发性有机溶剂在1.0~20 μg/kg、酯类10~200 μg/kg、酮类100~2000 μg/kg、醇类500~10000 μg/kg添加范围内的平均添加回收率为61.0%~113.1%,相对标准偏差为1.9%~9.8%。对于烷烃类、芳香烃类和醚类挥发性有机溶剂的检出限为1.0 μg/kg、酯类10 μg/kg、酮类100 μg/kg、醇类500 μg/kg。该方法操作简单、快速,灵敏度和准确度高,适用于蜂蜜样品中多种挥发性有机溶剂残留量的同时检测。 相似文献
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A systematic approach for the identification and quantification of organic volatile impurities (OVIs) in pharmaceutical excipients is described. Analytical procedures utilizing static headspace capillary gas chromatography coupled with flame-ionization and MS detection techniques were developed for the analysis of toxic ICH class 1 solvents and US Pharmacopeia OVIs at sub-ppm levels, and commonly used organic solvents in a wide range of concentrations. Chromatographic conditions and headspace parameters for the methods were optimized for separation, sensitivity, and speed. The proposed methodologies were demonstrated to be selective, accurate, and reproducible, and were successfully applied to the rapid screening of OVIs in typical excipients. 相似文献
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Wang X Jiang T Yuan J Cheng C Liu J Shi J Zhao R 《Analytical and bioanalytical chemistry》2006,385(6):1082-1086
This paper demonstrates headspace liquid-phase microextraction (HS-LPME) as used for the determination of volatile residual
solvents in pharmaceutical products. This method is based on headspace liquid-phase microextraction capillary column gas chromatography.
Under optimum conditions, the linerary of the method ranged from 1 to 1,000 mg l−1. The limits of detection are 0.2–2.0 mg l−1 and relative standard deviations (RSD) for most of the volatile solvents were below 10%. This novel method is applied to
the analysis of volatile residual solvents in pharmaceutical products with satisfactory results. 相似文献
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A method for the identification of volatile organic compounds in packaging materials is presented in this study. These compounds are formed by thermooxidative degradation during the extrusion coating process in the manufacture of packaging. Headspace solid-phase microextraction (HS-SPME) was used as sample preparation technique prior to the determination of the volatile organic compounds by gas chromatography-mass spectrometry (GC-MS). The effects of extraction variables, such as the type of fibre, the incubation temperature, the pre-incubation time, the size of the vial and the extraction time on the amounts of the extracted volatile compounds were studied. The optimal conditions were found to be: carboxen-polydimethylsiloxane 75 microm fibre, 5 min of pre-incubation time, 100 degrees C of incubation temperature, 20-ml vial, and 15 min of extraction time. The chromatograms obtained by HS-SPME and static headspace extraction were compared in order to show that the HS-SPME method surpasses the static headspace method in terms of sensitivity. Twenty-five compounds were identified including carbonyl compounds (such as 3-methyl-butanal, 3-heptanone or octanal), carboxylic acids (such as pentanoic acid or hexanoic acid) known as odour causing compounds and hydrocarbons (such as decane, undecane or dodecane). Finally, the method was applied to different packaging samples (one odour-unacceptable, two odour-acceptable, and three odourless samples) and to the raw materials in order to find out the odour-responsible volatile organic compounds and their source. 相似文献
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顶空-气相色谱法进展 总被引:17,自引:0,他引:17
回顾了顶空采样气相色谱分析法在复杂基质中挥发性成分中的应用.总结并详述了顶空分析的三种重要模式-介绍了顶空分析的相关原理和整个顶空分析系统的参数优化过程.综述了顶空.气相色谱分析在生物样本中挥发性有机物的测定、药品中有机残留溶剂的检测、聚合材料中挥发性有机物的分析、环境中有害的有机挥发性物质分析、挥发油分析和烟草分析等方面的进展. 相似文献
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气相色谱-串联质谱法测定皮革和纺织品中的富马酸二甲酯 总被引:5,自引:0,他引:5
建立了气相色谱-串联质谱(GC-MS/MS)准确、快速测定皮革和纺织品中富马酸二甲酯(DMF)的分析方法。样品经乙酸乙酯提取、浓缩及固相萃取柱净化处理,通过VF-5ms色谱柱分离、串联质谱对DMF进行定性和定量分析。实验结果表明: 优化样品预处理条件、固相萃取条件、质谱分析条件后,该方法可进一步消除杂质干扰,结果准确可靠,灵敏度、精密度、线性关系良好,回收率较高。3种浓度水平的加标回收率(n=6)保持在84%~93%之间,相对标准偏差小于7.2%;DMF在8种皮革和纺织品中的检出限 (S/N=3)为0.012~0.039 mg/kg, 0.05~100 mg/L质量浓度范围内线性相关系数为0.9990,适用于皮革和纺织品中DMF的日常检测。 相似文献