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Determination of 8 Diuretics and Probenecid in Human Urine by Gas Chromatography-Mass Spectrometry: Confirmation Procedure 被引量:2
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作者 Olga Zaporozhets Iuna Tsyrulneva Mykola Ischenko 《American Journal of Analytical Chemistry》 2012年第4期320-327,共8页
A fast and sensitive method for determination of 8 diuretics (acetazolamide, bendroflumethiazide, bumetanide, chlorthalidone, furosemide, hydrochlorothiazide, metolazone, triamterene) and masking agent (probenecid) in... A fast and sensitive method for determination of 8 diuretics (acetazolamide, bendroflumethiazide, bumetanide, chlorthalidone, furosemide, hydrochlorothiazide, metolazone, triamterene) and masking agent (probenecid) in human urine using gas-chromatography with mass spectrometric detection is described. The extraction of the substances as function of the nature of organic solvent, mixing time and pH of aqueous phase was studied. The tandem mass spectrometry was used to increase selectivity of diuretics determination due to elimination of background interferences. Fragmentation reactions were studied for each compound and their collision energies were optimized to obtain the best selectivity. The results of method’s validation demonstrate its suitability in routine analysis for confirmation purposes. 展开更多
关键词 DIURETICS URINE gas chromatography Tandem mass spectrometry CONFIRMATION
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Analyzing crude oils from the Junggar Basin(NW China) using comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry(GC×GC-TOFMS) 被引量:1
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作者 Yuce Wang Wanyun Ma +2 位作者 Ni Zhou Jiangling Ren Jian Cao 《Acta Geochimica》 EI CAS CSCD 2017年第1期66-73,共8页
As a new technology of analyzing crude oils,comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry(GC×GCTOFMS) has received much research attention.Here we present a case s... As a new technology of analyzing crude oils,comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry(GC×GCTOFMS) has received much research attention.Here we present a case study in the Junggar Basin of NW China.Results show that the hydrocarbons,including saturates and aromatics,were all well-separated without large coelution,which cannot be realized by conventional one-dimensional GC-MS.The GC×GC technique is especially effective for analyzing aromatics and low-to-middlemolecular-weight hydrocarbons,such as diamondoids.The geochemical characteristics of crude oils in the study area were investigated through geochemical parameters extracted by GC×GC-TOFMS,improving upon the understanding obtained by GC-MS.Thus,the work here represents a new successful application of GC×GCTOFMS,showing its broad usefulness in petroleum geochemistry. 展开更多
关键词 Comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry(GC×GC-TOFMS) Petroleum geochemistry Biomarkers Diamondoid Junggar Basin
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Headspace Solid-Phase Micro-Extraction Gas Chromatography/Mass Spectrometry(HS-SPME-GC/MS)-Based Untargeted Metabolomics Analysis for Comparing the Volatile Components from 12 Panax Herbal Medicines 被引量:1
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作者 Simiao Wang Xiaohang Li +8 位作者 Meiting Jiang Xinlong Wu Yuying Zhao Meiyu Liu Xiaoyan Xu Huimin Wang Hongda Wang Heshui Yu Wenzhi Yang 《Phyton-International Journal of Experimental Botany》 SCIE 2022年第7期1353-1364,共12页
Quality control of ginseng currently is mainly based on ginsenoside analysis,but rarely focuses on the volatile organic components.In the current work,an untargeted metabolomics approach,by headspace solid-phase micro... Quality control of ginseng currently is mainly based on ginsenoside analysis,but rarely focuses on the volatile organic components.In the current work,an untargeted metabolomics approach,by headspace solid-phase micro-extraction gas chromatography/mass spectrometry(HS-SPME-GC/MS),was elaborated and further employed to holistically compare the compositional difference of the volatile components simultaneously from 12 Panax herbal medicines,which included P.ginseng(PG),P.quinquefolius(PQ),P.notoginseng(PN),red ginseng(PGR),P.ginseng leaf(PGL),P.quinquefolius leaf(PQL),P.notoginseng leaf(PNL),P.ginseng flower(PGF),P.quinquefolius flower(PQF),P.notoginseng flower(PNF),P.japonicus(PJ),and P.japonicus var.major(PJvm).Chromatographic separation was performed on an HP-5MS elastic quartz capillary column using helium as the carrier gas,enabling good resolution within 1 h.We were able to characterize totally 259 volatile compounds,including 82 terpenes(T),46 alcohols(Alc),29 ketones(K),25 aldehydes(Ald),21 esters(E),and the others.By analyzing 90 batches of ginseng samples based on the untargeted metabolomics workflows,236 differential ions were unveiled,and accordingly 36 differential volatile components were discovered.It is the first report that simultaneously compares the compositional difference of volatile components among 12 Panax herbal medicines,and useful information is provided for the quality control of ginseng aside from the well-known ginsenosides. 展开更多
关键词 Headspace solid-phase micro-extraction gas chromatography/mass spectrometry PANAX volatile component untargeted metabolomics
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Occurrence of <i>N</i>-Acyl Homoserine Lactones in Extracts of Bacterial Strain of <i>Pseudomonas aeruginosa</i>and in Sputum Sample Evaluated by Gas Chromatography–Mass Spectrometry 被引量:1
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作者 Susheela Rani Ashwini Kumar +1 位作者 Ashok Kumar Malik P. Schmitt-Kopplin 《American Journal of Analytical Chemistry》 2011年第2期294-302,共9页
This study presents a fast, accurate and sensitive technique using gas chromatography-mass spectrometry (GC-MS) for the identification and quantification of N-acyl homoserine lactones (AHLs) in the extracts of bacteri... This study presents a fast, accurate and sensitive technique using gas chromatography-mass spectrometry (GC-MS) for the identification and quantification of N-acyl homoserine lactones (AHLs) in the extracts of bacterial strain of Pseudomonas aeruginosa and sputum sample of a cystic fibrosis patient. This method involves direct separation and determination of AHLs by using GC-MS as simultaneous separation and characterization of AHLs were possible without any prior derivatiza-tion. Electron ionization resulted in a common fragmentation pattern with the most common fragment ion at m/z 143 and other minor peaks at 73, 57 and 43. The limit of detection for N-butanoyl, N-hexanoyl, N-octanoyl, N-decanoyl, N-dodecanoyl and N-tetradecanoyl homoserine lactones was 2.14, 3.59, 2.71, 2.10, 2.45 and 2.34 μg/L, respectively. The presence of AHLs in the culture of P. aeruginosa strain and spu-tum of a cystic fibrosis patient was achieved in selected ion monitoring (SIM) mode by using the prominent fragment at m/z 143. 展开更多
关键词 gas chromatographymass spectrometry N-Acyl HOMOSERINE LACTONE (N-Butanoyl N-Hexanoyl N-Octanoyl N-Decanoyl N-Dodecanoyl and N-Tetradecanoyl) HOMOSERINE LACTONE SPUTUM Sample Bacterial Strain
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Structure Elucidation of a New Toxin from the Mushroom Cortinarius rubellus Using Gas Chromatography-Mass Spectrometry (GC-MS)
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作者 Ilia Brondz 《International Journal of Analytical Mass Spectrometry and Chromatography》 2013年第2期109-118,共10页
Cortinarius orellanus (Fries) and C. rubellus (Cooke),which were formerly also known as C. speciosissimus, are poisonous mushrooms containing the toxin orellanine and several degradation products of orellanine,includi... Cortinarius orellanus (Fries) and C. rubellus (Cooke),which were formerly also known as C. speciosissimus, are poisonous mushrooms containing the toxin orellanine and several degradation products of orellanine,includingorelline and orellinine. Mass intoxication by poisonous mushrooms was observed in Poland in 1952-1957 [1]. In 1957, the cause of these outbreaks was described by Grzymala as poisoning by a member of the Cortinarius family. The toxin orellanine was first isolated from C. orellanusby Grzymala in 1962;the chemical structure of orellanine was later determined to be 3,3',4,4'-tetrahydroxy-2,2'-bipyridine-N,N'-dioxide. Poisoning with C. orellanus and C. rubellus has a very specific character. The first symptoms of intoxication usually do not appear until 2-3 days after ingestion, but in some cases intoxication appears after three weeks. The target organ for the toxin is the kidney. Histologically, it is easy to record the specific damage. The presence of degradation products of orellanine in kidney can be confirmed chromatographically, suggesting that the cause of poisoning is orellanine. However, the presence of orellanine in the blood of intoxicated persons has not been directly detected. A specific model was developed by Brondz et al. for the detection of orellanine, orelline, and orellininein animal stomach fluids [2-4]. The hypothesis that the fungal toxin orellanine as a diglucoside can be transported from the digestive system by the blood to the kidney could not be supported. The toxin orellanine as a diglucoside is very unstable in an aqueous acidic environment.[i1]?However, in the present study, it was possible to record an additional substance in animal stomach fluids using GC-MSafter ingestion ofC. rubellus. This substance, which has been namedrubelline, is part of a toxic mixture inC. orellanusandC. rubellusand is closely related to orellanine. The structure of rubelline is more suitable than orellanine for absorptionfromthe digestive tract and for transport in the blood. The presented hypothesis is that rubellineis absorbed in the digestive tract and transportedin the blood to the kidney, where it is biotransformed to orellanine and accumulatedto toxic levels. The process of biotransformationis in itself also damaging for the kidney and liver.[i2]?GC-MS instrumentation enables the separation of substances in biological samples and in the extract fromC. rubellus. The GC-MS with SMB technique was used to record the mass ion and to record a detailed fragmentation picture. 展开更多
关键词 gas chromatography mass spectrometry
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The Detection of THCA Using 2-Dimensional Gas Chromatography-Tandem Mass Spectrometry in Human Fingernail Clippings: Method Validation and Comparison with Head Hair
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作者 Joseph Jones Mary Jones +1 位作者 Charles Plate Douglas Lewis 《American Journal of Analytical Chemistry》 2013年第10期1-8,共8页
Marijuana use as well as abuse is a significant public health and public safety concern in the United States and using hair to identify marijuana users and abusers has been gaining acceptance in a number of venues inc... Marijuana use as well as abuse is a significant public health and public safety concern in the United States and using hair to identify marijuana users and abusers has been gaining acceptance in a number of venues including workplace, court ordered, and substance abuse treatment monitoring. After the presentation of a fully validated 2-dimensional gas chromatography-tandem mass spectrometry method for the detection of 11-nor-9-carboxy-Δ9-tetrahydrocannabinol (THCA), the chief metabolite of the main psychoactive compound in marijuana, Δ9-tetrahydrocannabinol (THC), we evaluated the usefulness of fingernail clippings as an alternative specimen type to hair by the analysis of a set of 60 matched pairs of head hair and fingernail clippings. The limit of detection was 10 fg/mg, the limit of quantitation was 20 fg/mg, and the assay was linear from 20 fg/mg to 500 fg/mg. The intra- and inter-assay imprecision and bias studies at 4 different concentrations (50, 100, 500, and 1000 fg/mg) were acceptable where all % Target observations were within 16% of their expected concentrations and all %CV calculations were less than 13.5%. THCA was detectable in more fingernail specimens (53.3%) than hair specimens (46.7%) and the mean concentrations in nails were on average 4.9 times higher than in hair (1813 fg/mg and 364 fg/mg, respectively). The THCA concentrations in hair and nail were strongly associated (r = 0.974, P < 0.01, n = 60) and the association was significant. The study demonstrated that fingernail clippings are a suitable alternative specimen type to hair to monitor for marijuana use and abuse. 展开更多
关键词 11-Nor-9-Carboxy-Δ9-Tetrahydrocannabinol THCA Carboxy-THC HAIR Fingernail 2D-GC-MS/MS 2-Dimensional gas chromatography Tandem mass spectrometry
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Metabolomics of gastric cancer metastasis detected by gas chromatography and mass spectrometry 被引量:12
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作者 Jin-Lian Chen,Jun-Duo Hu,Jing Fan,Jing Hong,Department of Gastroenterology,Shanghai Sixth People’s Hospital,Shanghai Jiao Tong University,Shanghai 200233,China Hui-Qing Tang,Jian-Zhong Gu,Shanghai Laboratory Animal Center,Chinese Academy of Sciences,Shanghai 201615,China 《World Journal of Gastroenterology》 SCIE CAS CSCD 2010年第46期5874-5880,共7页
AIM:To elucidate the underlying mechanisms of metastasis and to identify the metabolomic markers of gastric cancer metastasis.METHODS:Gastric tumors from metastatic and nonmetastatic groups were used in this study.Met... AIM:To elucidate the underlying mechanisms of metastasis and to identify the metabolomic markers of gastric cancer metastasis.METHODS:Gastric tumors from metastatic and nonmetastatic groups were used in this study.Metabolites and different metabolic patterns were analyzed by gas chromatography,mass spectrometry and principal components analysis (PCA),respectively.Differentiation performance was validated by the area under the curve (AUC) of receiver operating characteristic curves.RESULTS:Twenty-nine metabolites were differentially expressed in animal models of human gastric cancer.Of the 29 metabolites,20 were up-regulated and 9 were down-regulated in metastasis group compared to non-metastasis group.PCA models from the metabolite profiles could differentiate the metastatic from the nonmetastatic specimens with an AUC value of 1.0.These metabolites were mainly involved in several metabolic pathways,including glycolysis (lactic acid,alaline),serine metabolism (serine,phosphoserine),proline metabolism (proline),glutamic acid metabolism,tricarboxylic acid cycle (succinate,malic acid),nucleotide metabolism (pyrimidine),fatty acid metabolism (docosanoic acid,and octadecanoic acid),and methylation(glycine).The serine and proline metabolisms were highlighted during the progression of metastasis.CONCLUSION:Proline and serine metabolisms play an important role in metastasis.The metabolic profiling of tumor tissue can provide new biomarkers for the treatment of gastric cancer metastasis. 展开更多
关键词 gasTRIC cancer METASTASIS METABOLITE Metabolomics gas chromatography and mass spectrometry
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Gas chromatography/mass spectrometry based metabolomic study in a murine model of irritable bowel syndrome 被引量:7
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作者 Lei-Min Yu Ke-Jia Zhao +2 位作者 Shuang-Shuang Wang Xi Wang Bin Lu 《World Journal of Gastroenterology》 SCIE CAS 2018年第8期894-904,共11页
AIM To study the role of microbial metabolites in the modulation of biochemical and physiological processes in irritable bowel syndrome(IBS).METHODS In the current study, using a metabolomic approach, we analyzed the ... AIM To study the role of microbial metabolites in the modulation of biochemical and physiological processes in irritable bowel syndrome(IBS).METHODS In the current study, using a metabolomic approach, we analyzed the key metabolites differentially excreted in the feces of control mice and mice with IBS, with or without Clostridium butyricum(C. butyricum) treatment. C57 BL/6 mice were divided into control, IBS, and IBS + C. butyricum groups. In the IBS and IBS + C. butyricum groups, the mice were subjected to water avoidance stress(WAS) for 1 h/d for ten days. Gas chromatography/mass spectrometry(GC-MS) together with multivariate analysis was employed to compare the fecal samples between groups. RESULTS WAS exposure established an appropriate model of IBS in mice, with symptoms of visceral hyperalgesia and diarrhea. The differences in the metabolite profiles between the control group and IBS group significantly changed with the progression of IBS(days 0, 5, 10, and 17). A total of 14 differentially excreted metabolites were identified between the control and IBS groups, and phenylethylamine was a major metabolite induced by stress. In addition, phenylalanine metabolism was found to be the most relevant metabolic pathway. Between the IBS group and IBS + C. butyricum group, 10 differentially excreted metabolites were identified. Among these, pantothenate and coenzyme A(Co A) biosynthesis metabolites, as well as steroid hormone biosynthesis metabolites were identified as significantly relevant metabolic pathways.CONCLUSION The metabolic profile of IBS mice is significantly altered compared to control mice. Supplementation with C. butyricum to IBS mice may provide a considerable benefit by modulating host metabolism. 展开更多
关键词 IRRITABLE BOWEL syndrome METABOLITE gas chromatography/mass spectrometry CLOSTRIDIUM butyricum
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ANALYSIS OF VOLATILE CONSTITUENTS OF CHINESE MEDICINAL HERBS BY FLASH DISTILLATION/CAPILLARY GAS CHROMATOGRAPHY/MASS SPECTROMETRY
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《Chemical Research in Chinese Universities》 SCIE CAS 1986年第1期13-18,共6页
In present work,the volatile constituents of Curcuma longa L.,A.lancea (Thunb.) DC.,Foeniculum vulgare Mill,and Cinnamomun cassia Presl.have been analyzed by flash distillation/capillary gas chro-matography/mass spect... In present work,the volatile constituents of Curcuma longa L.,A.lancea (Thunb.) DC.,Foeniculum vulgare Mill,and Cinnamomun cassia Presl.have been analyzed by flash distillation/capillary gas chro-matography/mass spectrometry.The results are consistent with those obtained by conventional steam distillation extraction method.The optimum condition of flash distillation has been studied.The experimental results showed that this new technique proved to be a simple,rapid and efficient tool for microanalysis of volatile constituents of Chinese medicinal herbs. 展开更多
关键词 OC ANALYSIS OF VOLATILE CONSTITUENTS OF CHINESE MEDICINAL HERBS BY FLASH DISTILLATION/CAPILLARY gas chromatography/mass spectrometry gas
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生物样品中聚苯乙烯纳米塑料指示物的热裂解-气相色谱质谱检测方法研究
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作者 谢颖 李明姣 +4 位作者 杨波 张少平 董小艳 王琼 唐宋 《环境卫生学杂志》 2024年第6期501-507,共7页
目的采用热裂解-气相色谱质谱法(Py-GC/MS)建立一种从生物组织样品中定量测定纳米级聚苯乙烯(PS)塑料的方法。方法通过比较和优化不同消解液、蛋白沉淀剂以及仪器检测参数体系,确定生物样品中PS塑料的最优前处理和检测方法。通过开展实... 目的采用热裂解-气相色谱质谱法(Py-GC/MS)建立一种从生物组织样品中定量测定纳米级聚苯乙烯(PS)塑料的方法。方法通过比较和优化不同消解液、蛋白沉淀剂以及仪器检测参数体系,确定生物样品中PS塑料的最优前处理和检测方法。通过开展实验研究确定方法特性指标(包括检出限、定量限、精密度和准确度),并基于方法开展了实际样品测定。结果本研究建立了大鼠肝和肺组织样本经10%氢氧化钾溶液消解和无水乙醇蛋白沉淀后上Py-GC/MS检测的方法,PS在0.05~2.00μg范围内线性关系良好,相关系数为0.999,检出限和定量限分别为0.012和0.036μg/g,且当添加水平为低浓度(2μg/g)、中浓度(10μg/g)、高浓度(30μg/g)PS时,其加标回收率分别为68.0%~85.0%、80.0%~105%和62.0%~93.1%,精密度(RSD)范围在7.8%~15.2%。结论本研究建立的方法满足方法学要求,且为其他生物样本及其他类型微塑料的检测提供了参考,为进一步开展纳米塑料的人群内暴露水平研究和健康风险评估奠定了技术基础。 展开更多
关键词 热裂解-气相色谱质谱法 生物组织 纳米塑料
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基于自动质谱解卷积与识别系统-气相色谱质谱技术筛查分析聚乳酸餐盒可迁移添加剂
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作者 王建凤 赵青原 +5 位作者 殷佩珊 陈婷 王佳敏 史迎杰 刘艳 高峡 《食品安全质量检测学报》 CAS 2024年第13期19-28,共10页
目的 基于自动质谱解卷积与识别系统-气相色谱质谱技术筛查聚乳酸餐盒中可迁移添加剂。方法 采用傅里叶变换红外光谱法(Fourier transform infrared,FTIR)结合热裂解/气相色谱-质谱法(pyrolysis-gas chromatography mass spectrometry,P... 目的 基于自动质谱解卷积与识别系统-气相色谱质谱技术筛查聚乳酸餐盒中可迁移添加剂。方法 采用傅里叶变换红外光谱法(Fourier transform infrared,FTIR)结合热裂解/气相色谱-质谱法(pyrolysis-gas chromatography mass spectrometry,Py-GC-MS)对餐盒材质鉴定,并将餐盒置于不同模拟液和不同温度进行迁移实验,GC-MS进行检测,基于自动质谱解卷积与识别系统(automated mass spectral deconvolution and identification system,AMDIS)及自研数据处理程序MSData批量处理数据,分析可迁移添加剂,并利用标准品和保留指数验证。结果 所售餐盒的材质为聚乳酸,AMDIS、谱库检索和结果 验证能够显著提高可迁移添加剂鉴定的准确性,MSData可提升数据处理效率,共筛查出18种可迁移添加剂,其中4℃可以迁移出的添加剂只有6种,随温度升高,在25℃条件下新增4种,70℃条件下新增8种。经毒性预测,9种低毒,8种微毒,1种无毒;其中11种呈现出微弱的发育毒性;致畸性均为阴性。结论 该分析方法 快速、方便,可推广至其他聚乳酸餐盒中可迁移添加剂的快速筛查分析。 展开更多
关键词 聚乳酸 添加剂 迁移 自动质谱解卷积与识别系统 热裂解
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Analysis of residual crosslinking agent content in UV cross-linked poly(ethylene oxide) hydrogels for dermatological application by gas chromatography 被引量:1
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作者 Rachel Shet Hui Wong Mark Ashton Kalliopi Dodou 《Journal of Pharmaceutical Analysis》 SCIE CAS 2016年第5期307-312,共6页
Acrylates have been widely used in the synthesis of pharmaceutical polymers. The quantitation of residual acrylate monomers is vital as they are strong irritants and allergens, but after polymerization, are relatively... Acrylates have been widely used in the synthesis of pharmaceutical polymers. The quantitation of residual acrylate monomers is vital as they are strong irritants and allergens, but after polymerization, are relatively inert, causing no irritation and allergies. Poly(ethylene oxide)(PEO) hydrogels were prepared using pentaerythritol tetra-acrylate(PETRA) as UV crosslinking agent. A simple, accurate, and robust quantitation method was developed based on gas chromatographic techniques(GC), which is suitable for routine analysis of residual PETRA monomers in these hydrogels. Unreacted PETRA was initially identified using gas chromatography–mass spectrometry(GC–MS). The quantitation of analyte was performed and validated using gas chromatography equipped with a flame ionization detector(GC–FID). A linear relationship was obtained over the range of 0.0002%–0.0450%(m/m) with a correlation coefficient(r2)greater than 0.99. The recovery( 4 90%), intra-day precision(%RSD o 0.67), inter-day precision(%RSD o2.5%), and robustness(%RSD o1.62%) of the method were within the acceptable values. The limit of detection(LOD) and limit of quantitation(LOQ) were 0.0001%(m/m) and 0.0002%(m/m), respectively.This assay provides a simple and quick way of screening for residual acrylate monomer in hydrogels. 展开更多
关键词 Poly(ethylene oxide) (PEO) RESIDUAL MONOMER Hydrogelgas chromatographymass spectrometry (GC–MS) gas chromatography–flame ionization detection (GC–FID)
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热裂解-气质联用仪(PY-GC/MS)在微塑料分析中的应用
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作者 陈智 杨荞安 +1 位作者 张娜 谢依侨 《当代化工》 CAS 2024年第5期1198-1207,1232,共11页
塑料是一种合成材料,因其成本低廉、耐用、重量轻、易于制造等众多优点,使得这些聚合物在日常生活中无处不在。近年来,科学家、环保部门和公众越来越关注塑料污染,特别是微/纳米塑料。通常,研究各类样品中的微塑料都需要从样品中将微塑... 塑料是一种合成材料,因其成本低廉、耐用、重量轻、易于制造等众多优点,使得这些聚合物在日常生活中无处不在。近年来,科学家、环保部门和公众越来越关注塑料污染,特别是微/纳米塑料。通常,研究各类样品中的微塑料都需要从样品中将微塑料颗粒分离出来,然后用光谱方法来识别分析。光谱技术可进行微塑料的定性分析,但无法获取其准确的质量,而这些对毒理学评估很重要。为了同时实现样品中微塑料的定性和定量分析,许多研究人员开始进行热裂解-气相色谱/质谱法(PY-GC/MS)在微塑料分析中的应用。综述了近5年PY-GC/MS在微塑料研究中的应用,包括PY-GC/MS技术简介、样品采集、样品前处理、仪器分析方法建立以及问题与展望。 展开更多
关键词 微塑料 热裂解-气相色谱/质谱法 定量分析
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热裂解-气相色谱-质谱联用法测定生物降解塑料制品中PBAT含量的方法
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作者 郗丹 范秀凯 +5 位作者 唐孔科 齐永润 徐正 赵英杰 李林林 潘庆燕 《青岛科技大学学报(自然科学版)》 CAS 2024年第3期81-86,共6页
采用热裂解-气相色谱-质谱联用法对生物基降解塑料制品中生物基降解材料聚己二酸/对苯二甲酸丁二酯(PBAT)定性定量分析;选用二氯甲烷为生物降解塑料材料制品的溶剂,通过对生物降解材料PBAT的热裂解温度,气质试验参数,标准物质筛选,特征... 采用热裂解-气相色谱-质谱联用法对生物基降解塑料制品中生物基降解材料聚己二酸/对苯二甲酸丁二酯(PBAT)定性定量分析;选用二氯甲烷为生物降解塑料材料制品的溶剂,通过对生物降解材料PBAT的热裂解温度,气质试验参数,标准物质筛选,特征碎片的确定及多组分检测干扰因素排查,确定了PBAT裂解特征产物1,6-二氧杂环十二烷-7,12-二酮和苯甲酸,采用二者峰面积之和进行定量。在10~500 mg·L^(-1)内具有良好的线性关系,且在10、50、250 mg·L^(-1)3种添加水平下的回收率在90.7%~97.9%,相对标准偏差在10%以内,稳健度符合要求。 展开更多
关键词 热裂解-气相色谱-质谱联用 生物可降解塑料及制品 聚己二酸/对苯二甲酸丁二醇酯(PBAT)
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Coupling a Gas Chromatography Unit to an Inductively Coupled Plasma Mass Spectrometer
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作者 Jerrad P. Auxier John D. Auxier II Howard L. Hall 《World Journal of Nuclear Science and Technology》 2017年第2期84-92,共9页
Although the eminent threat of a terrorist group detonating an improvised nuclear device (IND) in an urban environment is low, it is crucial that countries develop modern nuclear forensic capabilities to expedite resp... Although the eminent threat of a terrorist group detonating an improvised nuclear device (IND) in an urban environment is low, it is crucial that countries develop modern nuclear forensic capabilities to expedite response in a post-detonation scenario. In particular, new instruments need to be created to shorten dissolution time, expedite chemical separation, and improve forensic analysis of the nuclear melt glass that is created during the detonation of the device. To expedite this process, an instrument was designed to thermally couple a gas chromatograph (GC) to a time-of-flight inductively coupled plasma time-of-flight mass spectrometer (ICPTOFMS) In order to couple these two instruments, another instrument was designed to provide an isothermal atmosphere between the GC and TOFICPMS to expedite rapid gas separations processes. By using gas separations instead of the current wet chemistry processes, the required separation and analysis time of the melt glass significantly decreases. The new instrument would also provide a more detailed analysis of the elemental and isotopic composition of the melt glass. By completing these tasks simultaneously, this significantly decreases the required time to conduct these separations and improves the elemental and isotopic analysis. 展开更多
关键词 NUCLEAR FORENSICS gas chromatography mass spectrometry Melt Glass Chemical Separation NUCLEAR Security ELEMENTAL Analysis
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热裂解-气相色谱-质谱法鉴别生物可降解塑料 被引量:6
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作者 王利敏 程森祥 +1 位作者 宋晓宇 陈彤 《理化检验(化学分册)》 CAS CSCD 北大核心 2023年第3期297-302,共6页
目前生物可降解塑料主要采用堆肥降解测定其生物降解性能的方法进行鉴别,其检测周期长、费用较高。材料的组成基本决定了其生物降解特性,为了快速鉴别生物可降解塑料,采用热裂解-气相色谱-质谱法(PY-GC-MS)对以聚对苯二甲酸-己二酸丁二... 目前生物可降解塑料主要采用堆肥降解测定其生物降解性能的方法进行鉴别,其检测周期长、费用较高。材料的组成基本决定了其生物降解特性,为了快速鉴别生物可降解塑料,采用热裂解-气相色谱-质谱法(PY-GC-MS)对以聚对苯二甲酸-己二酸丁二醇酯(PBAT)与不同质量比的其他成分包括生物可降解聚乳酸(PLA)、难降解材料聚苯乙烯(PS)或聚对苯二甲酸乙二醇酯(PET)混合样的裂解特征进行了研究。结果显示,PBAT的裂解特征峰明显,未受到PLA的影响;若在PBAT中添加质量分数1%的非降解材质PS和PET也可被检出。方法用于市场上收集到的标识为可降解塑料购物袋样品的分析,结果表明,采用PY-GC-MS可以快速对可降解塑料进行初步鉴别。 展开更多
关键词 热裂解-气相色谱-质谱法(PY-GC-MS) 生物可降解塑料 聚对苯二甲酸-己二酸丁二醇酯(PBAT)
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中国东北干旱-半干旱地区湖泊沉积物木质素酚类化合物特征及其气候指示意义 被引量:1
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作者 尚文郁 孙青 +1 位作者 谢曼曼 战楠 《岩矿测试》 CAS CSCD 北大核心 2023年第2期346-360,共15页
木质素广泛分布于维管植物,经分解生成的酚类化合物可示踪有机质来源、评估木质素降解程度,进而用于反演古环境与古气候变化。采用合适的分析方法有效地分解木质素是推断母源植物类型、降解程度的技术基础,常规方法是木质素经碱(或酸)解... 木质素广泛分布于维管植物,经分解生成的酚类化合物可示踪有机质来源、评估木质素降解程度,进而用于反演古环境与古气候变化。采用合适的分析方法有效地分解木质素是推断母源植物类型、降解程度的技术基础,常规方法是木质素经碱(或酸)解后,利用气相色谱-质谱法(GC-MS)分析酚类单体化合物,但分解、提取过程复杂、易引入杂质。热裂解技术可在高温下快速分解有机质,裂解产物可通过GC-MS进行在线分析,具有用样量少、有机质提取比例高、重现性好、操作便捷的特点。本文选择地处亚洲夏季风影响区域的边缘的内蒙伊和沙日乌苏湖,采用热裂解GC-MS(Py-GC/MS)技术,对湖泊沉积物进行裂解分析,在对裂解温度(450℃、550℃和650℃)进行了优化的基础上,识别了21种酚类化合物,包括:4-甲基苯酚、2-乙基苯酚等9种烷基酚类(PHs),4-乙基-2-甲氧基苯酚、4-乙烯基-2,6-二甲氧基苯酚等9种烷基酚类(PHs)和12种甲氧基酚类(LGs)。结合沉积岩心样品AMS 14 C年龄的分析结果,6.7 ka以来沉积物中酚类化合物总量、PHs和LGs的变化趋势总体一致,呈现出6.7~4.0ka相对含量较高、4.0ka以来相对含量较低的特征。不同于PHs中邻(o-)-PHs、间(m-)-PHs、对(p-)-PHs的变化趋势与总量一致;但不同取代特征的LGs相对含量变化趋势存在差异,p-LGs在5.4ka前后就出现含量显著下降,3.8ka以来维持较低水平。根据微生物对木质素的“去甲基/去甲氧基”氧化反应途径,对位取代酚类化合物比值(p-PHs/p-LGs)可作为陆生高等植物降解指标,该值越大微生物降解作用越强。将p-PHs/p-LGs指标应用于伊和沙日乌苏沉积物样品结果显示,6.7ka以来p-PHs/p-LGs与正构烷烃单体碳同位素δ^(13) C_(27-33)变化趋势一致(R=-0.77),间接地指示了有效降水变化。即6.7ka以来气候整体转湿,区内陆生高等植物占据优势,充足的水分和有机质为微生物提供了适宜的生存环境和相对稳定的营养来源,降解作用整体呈增强趋势;6.3~5.5ka和4.1~3.6ka期间有效湿度降低,微生物对木质素的降解作用相对减弱。p-PHs/p-LGs指标对应了呼伦贝尔地区湿度变化特征,揭示了干旱-半干旱地区微生物降解与有效湿度变化的相关性,为探讨陆地生态系统对东亚季风北部边缘区气候变化的响应提供科学依据。 展开更多
关键词 热裂解-气相色谱-质谱法 伊和沙日乌苏湖 木质素酚类单体化合物 微生物降解 古气候
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基于热裂解-气相色谱-质谱法和随机森林的加热卷烟烟叶原料适用性评估 被引量:2
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作者 陈颐 范迎杰 +3 位作者 汪旭 杨菁 赵文涛 张志敏 《理化检验(化学分册)》 CAS CSCD 北大核心 2023年第1期21-28,共8页
基于热裂解-气相色谱-质谱法(Py-GC-MS)和随机森林(RF),从化学成分角度分析加热卷烟烟叶原料适用性。称取过筛后的样品粉末0.90 mg于样品杯中,采用Py-GC-MS对28种不同类型的加热卷烟进行检测,用MZmine软件对Py-GC-MS数据进行处理,获得... 基于热裂解-气相色谱-质谱法(Py-GC-MS)和随机森林(RF),从化学成分角度分析加热卷烟烟叶原料适用性。称取过筛后的样品粉末0.90 mg于样品杯中,采用Py-GC-MS对28种不同类型的加热卷烟进行检测,用MZmine软件对Py-GC-MS数据进行处理,获得含有峰强度信息的特征峰表。分别以样品的特征峰表和感官评价得分作为自变量和因变量,采用RF回归算法建立加热卷烟烟叶原料适用性模型。结果显示:RF模型在训练集上的决定系数为0.93,均方根误差为0.85,在测试集上的决定系数为0.92,均方根误差为0.96;根据NIST 2017库的定性结果,共筛选出20个特征重要性评分较高的化学成分。 展开更多
关键词 加热卷烟 热裂解-气相色谱-质谱法 随机森林 化学成分
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基于TGA和Py-GC/MS不同成熟度煤的热解特征研究
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作者 李美菊 操涛 +4 位作者 邹春林 范行军 宋建中 于赤灵 彭平安 《地球化学》 CAS CSCD 北大核心 2023年第4期428-438,共11页
采用热重分析(TGA)和热解–气相色谱/质谱(Py-GC/MS)联用技术对6个不同成熟度煤的热解过程及热解产物进行表征。TGA结果表明,不同成熟度煤的失重(TG)曲线具有相似性且在失重速率(DTG)曲线中有3个明显的失重速率峰;随着成熟度的增加,煤... 采用热重分析(TGA)和热解–气相色谱/质谱(Py-GC/MS)联用技术对6个不同成熟度煤的热解过程及热解产物进行表征。TGA结果表明,不同成熟度煤的失重(TG)曲线具有相似性且在失重速率(DTG)曲线中有3个明显的失重速率峰;随着成熟度的增加,煤在最高热解温度时的总失重率(wt)减小,最大失重速率(−(dw/dt)max)降低,但最大失重速率峰温度(Tmax)升高,说明低成熟度煤中热不稳定结构的含量较高。Py-GC/MS结果表明,不同成熟度煤的热解产物均以芳香类化合物为主(47.4%~94.7%),且芳香类热解产物的含量随成熟度的增加逐渐升高,说明高成熟度煤热解过程中产生的芳香类化合物较多,而热解产物中酚类、呋喃类和脂肪烃类化合物的占比随煤样成熟度的增加逐渐降低,表明低成熟度煤在热解过程中释放出高含量的极性含氧化合物。研究结果对进一步了解煤炭资源的规模化开发和合理利用具有重要意义。 展开更多
关键词 成熟度 热重分析 热解–气相色谱/质谱
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Pyrolysis Study of Waterborne Polyurethane
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作者 张燕红 《Journal of Wuhan University of Technology(Materials Science)》 SCIE EI CAS 2010年第3期479-483,共5页
The thermal degradation of synthetic waterborne polyurethane(PU) based on toluenediisocyanate(TDI) was investigated by pyrolysis-gas chromatography/mass spectrometry(Py-GC/MS) and thermogravimetry(TG).The degr... The thermal degradation of synthetic waterborne polyurethane(PU) based on toluenediisocyanate(TDI) was investigated by pyrolysis-gas chromatography/mass spectrometry(Py-GC/MS) and thermogravimetry(TG).The degradation profiles of cast films obtained from dispersions were evaluated.More than 20 characteristic volatile pyrolyzates reflecting the structure and pyrolysis mechanisms of the polymer have been identified by on-line MS.In helium atmosphere,the synthesized products of polyurethane were pyrolyzed at 350,450,550,650 and 750 ℃ respectively,and the thermal decomposition products were analyzed on line using GC/MS.The product analysis reveals that the pyrolyzates distribution of the polyurethane depends strongly on the pyrolysis temperature.Based on the Py-GC/MS data,the thermal degradation mechanism of the polyurethane is discussed. 展开更多
关键词 waterborne polyurethane pyrolysis-gas chromatography mass spectrometry pyrolysis THERMOGRAVIMETRY
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