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毛细管气相色谱,色谱—质谱联用测定金刚烷及其异构体 总被引:3,自引:0,他引:3
本文给出了金刚烷及其异构体合物系毛细管气相色谱及色谱-质谱联用分析方法,色谱柱为CBPI键合石英毛细管、氢火焰检则器。列出了标准曲线和检测条件,回收率为98.3%-101.2%,相对标准偏差〈4.0%,本方法定量分析快速、简便、准确。 相似文献
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基质固相分散和气相色谱-质谱法测定浓缩苹果汁中22种有机氯农药和15种拟除虫菊酯农药的残留量 总被引:36,自引:8,他引:28
建立了浓缩苹果汁样品中22种有机氯农药和15种拟除虫菊酯类农药的气相色谱-质谱检测方法。采用基质固相分散技术进行样品前处理,用气质联用仪在选择离子监测模式下进行快速定性定量分析,以双柱法对定性结果进行确认。研究了一定浓度范围内农药峰面积与浓度的线性关系,相关系数均好于0.99。除六氯苯外其余36种农药的添加回收率在70.4%~108.3%的范围内,相对标准偏差在2.1%~24.9%。 相似文献
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气相色谱/质谱法测定卷烟烟气中的主要挥发酸 总被引:7,自引:0,他引:7
以异丙醇为溶剂,壬醇为内标,采用气相色谱/质谱法定性定量分析了卷烟烟气中的游离态甲酸和乙酸,还测定了该方法的精密度和准确度,结果为:RSD小于2%,回收率大于97%. 相似文献
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本文用高压液相色谱对海豹油的主要组分进行定性、定量分析;利用气相色谱-质谱联用仪定性分析了海豹油脂中的脂肪酸部分,并以硬脂酸为内标,用气相色谱方法对海豹油脂肪酸各组分进行了定量分析,分析结果表明海豹油中油脂部分占92%,烯醛类气味物质占6%;海豹油脂中不饱和脂肪酸占脂肪酸总量的82%以上,而且富含γ-亚麻酸。为开发海豹油,从海豹油中分离除去其中气味物质-烯醛类方法的选择提供了依据。 相似文献
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烟草制品中紫苏葶的气相色谱/质谱法分析 总被引:1,自引:0,他引:1
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%. 相似文献
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复方祛风湿止痛药粉末中挥发性成分的静态顶空-气相色谱-质谱分析 总被引:3,自引:0,他引:3
利用静态顶空-毛细管气相色谱-质谱方法对复方祛风湿止痛药中挥发性成分进行了分析,运用质谱检索和保留指数对其中主要的60种挥发性成分进行了定性.该药中各种挥发性成分的相对含量分别为萜类(54.5%)、萜类衍生物(9.6%)、酚醚类(15.0%)和脂肪醇醛(8.5%),主要为β-古芸烯(20.5%)、蒿脑(14.5%)、β-蛇床烯(6.0%)和β-绿叶烯(5.7%).分析结果的相对标准偏差(RSD)在0.54%~8.39%之间. 相似文献
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M. Muruganandham 《Analytical letters》2017,50(6):916-923
Here are reported two new sampling method approaches for the determination of naphthalene in ambient air for concentrations from 0.25 to 18.7?µg/L. The first method used for gas phase naphthalene analysis produced an average recovery of 88.8% and the second method using headspace sampling produced an average recovery of 93.8%. The second method showed better recovery than the former, so it was used for subsequent comparative gas-phase determination of naphthalene. The second method was validated at various naphthalene concentrations and humidity using a naphthalene gas generator to produce various naphthalene standards and a naphthalene-monitoring instrument. The naphthalene concentrations generated using the gas generator and determined second sampling method with gas chromatography–mass spectrometry (GC–MS) were compared to the sensor measurements and were in good agreement. In summary, the sampling methods presented provided reliable gas-phase naphthalene determination when coupled with GC–MS. 相似文献
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采用GC/MS法检测出邻氰堪苄基氯中的杂质组分,并使用萘做内标物进行气相色谱法对邻氰堪苄基氯的定量检测。 相似文献
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An extremely simple and sensitive method was developed for determination of nitrated polycyclic aromatic hydrocarbons (nitro-PAHs; mono-nitro-PAHs and dinitropyrenes) in diesel exhaust particles (DEPs) by gas chromatography-negative ion chemical ionisation tandem mass spectrometry (GC/NCI/MS/MS). We used two types of column in GC/NCI/MS/MS analysis. A polar column was used for determination of mono-nitro-PAHs, and a non-polar column was used for determination of dinitropyrenes and mono-nitro-PAHs except nitrofluoranthenes. The proposed method requires no clean-up procedure. The limits of detection ranged from 0.01 to 0.09 pg for all compounds tested. The applicability of the method to DEP samples was validated using diesel particulate standard reference materials (SRMs). Although DEPs contain complex matrices, all compounds could be detected easily in SRM2975 (diesel particulate matter) and SRM1975 (diesel particulate extract) without a clean-up procedure. The RSDs were less than 5% for all compounds examined. The quantitative results for SRMs exhibited good agreement with the available data in the literature. These results indicate that the proposed GC/NCI/MS/MS method is useful for determination of nitro-PAHs in DEP samples. 相似文献
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A sensitive procedure for the determination of estrogens in urine has been developed, using enzymatic hydrolysis and ether extraction followed by capillary gas chromatography with negative chemical ionisation mass spectrometry (GC/NCI-MS) of the pentafluorobenzoyl derivatives. These derivatives were superior for GC/NCI-MS to trifluoroacetyl, heptafluorobutyl, pentadecafluorooctanoyl and perfluorotolyl derivatives, giving characteristic negative molecular ions as the base peak for each of the naturally occurring estrogens estrone, estradiol and estriol, and for the synthetic estrogen ethynylestradiol used in contraceptive pills. The method was also suitable for determination of some metabolites of estrone and estradiol. The specificity and sensitivity of the GC/NCI-MS method simplifies sample preparation. Recovery of spiked samples was in the range 84-101% for the natural estrogens based on additions to increase the concentration by 5 and 1 microg L(-1). The repeatability of the method was 1-8% for all estrogens. 相似文献
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A gas chromatographic (GC) method was developed for the determination of sucrose monoesters of fatty acids (mono-SuE) and sucrose acetate isobutyrate (SAIB) in food additive premixes. Mono-SuE and SAIB fractions were prepared by column chromatography with either a C8 or a silica gel solid-phase extraction column. The mono-SuE fraction was acetylated and applied to a wide-bore GC column (0.53 mm x 15 m) by splitless injection for determination. The SAIB fraction was applied to the GC column without derivatization. Gas chromatography/mass spectrometry was used to confirm the identity of GC peaks. The detection limits for mono-SuE and SAIB were 0.005 and 0.01%, respectively. Mono-SuE (C12, C14, C16, C18, and C18:1) and SAIB were found in commercial food additive premixes and some foods. 相似文献
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Determination of pesticide residues in lettuce by gas chromatography with electron-capture detection
A sensitive, rapid, and simple multiresidue method for the simultaneous determination of 19 pesticides in different varieties of lettuce (Lactuca sativum) was developed. Lettuce samples were extracted by homogenization with acetone and partitioned into ethyl acetate-cyclohexane. Subsequent sample cleanup was not needed. Final determination was made by capillary gas chromatography (GC) with electron-capture detection (ECD). Confirmation analysis of pesticides was performed by GC coupled with mass spectrometry in the selected ion monitoring mode. The average recovery by the GC-ECD method obtained for these compounds varied from 66.4 to 119.2% with relative standard deviations < 7.7%. The GC-ECD method has good linearity, and the detection limit for the pesticides studied varied from 0.1 to 3.8 microg/kg. The proposed method was used to determine pesticide levels in different types of lettuce grown in soils from experimental fields. 相似文献