GC/MS Analysis of Organic Compounds in Hot Water-Extractable Fraction from Shenfu Coal

Shenfu Coal was extracted with hot pure water and slurry was isolated. The concentrated benzene-soluble fraction (CBSF) was analyzed with GC/MS and four types of organic compounds (OCs) were detected: HACOCs,DTEs,DMDT and LCAs. The amount of benzyl benzoate which is the most abundant OC was calculated by an inter-nal standard method with an indicated amount of BP. The broken hydrogen bonds and ether bonds were responsible for the extraction of OCs from the coal .DTEs,DMDT and LCAs are essentially insoluble in water,whereas they are soluble,probably owing to intermolecular interaction of OCs with HACOCs.

LOCATION OF DOUBLE BOND POSITION OF INSECT SEX PHEROMONE BY GC/MS ANALYSIS WITH CHEMICAL IONIZATION

Ozonolysis products of four lepidopteral pheromone were identified by methane CI-MS.The spectra obtained were notably simpler than those of EI-MS,the peak of molecular ion was normally close to the base peak,and the characteristic fragment ions were high in m/z,thereby the interpretation was facilitated.

GC/MS Analysis of Fractional Extraction of Fusain from Tongting Bituminous Coal in CS_2

Fusain from Tongting (Huaibei, Anhui Province) bituminous (FTTB) coal was fractionally extracted using Soxhlet extractor with CS2. Then the extracts were analyzed with GC/MS. Comparison of experimental data between FTTB coal and clarain from Tongting bituminous (CTTB) coal was carried out. The results show that the kinds of small molecule components detected by GC/MS of FTTB are less than those of CTTB. Long-chain alkanes exist mostly in the extracts of fusain. Macromolecular networks are predominant in the FTTB coal mainly composed of inertinite in the coal petrography. The size of micropores in the FTTB coal is relatively small, and the development of micropores is relatively low. Thus the content of aromatic compounds with affinity for micropores is relative low in FTTB, while the content of long-chain alkanes with affinity for macromolecule networks is relatively high. Sub-components in exinite determine the distribution of long-chain alkanes extracted in the last stage. Odd-numbered carbon distribution appears when resin is most in exinite, while high carbon alkane distribution appears when exinite is dominant in cutinite. Small aromatic molecules are firstly packed in micropores, and exist in a free state after micropores are saturated.

GC/MS analyses of fractionated extraction of Shenfu coal with CS2,n-hexane,benzene

Shenfu coal was extracted with 0S2, n-hexane, benzene sequentially. The extracts were analyzed with GC/MS. It is presented that group seperation of soluble organic compounds in the coal can be achieved by fractionated extraction using different solvents. Main components in CS2 soluble fraction from Shenfu coal are alkyl-substituted arenes. Aliphatic hydrocarbons are overwhelmingly predominant in n-hexane-soluble fraction. Dito tricyclic aramatic hydrocarbons are identified in benzene-soluble fraction. The molecular structures detection of 2, 4, 6-trichlorobenzenamine and 3, 3＇, 4, 4＇, 5, 5＇-hexachloro-1, 1＇- biphenyl and 2-chlorocyclohexanol firstly provide information for existence form of chlorine in coal.

GC/MS Analysis of Long-Chain Aldehydes from Recent Coral

The main objective of this study is to present the chromatograms and mass spectra of aldehydes so that geochemists could easily identify these compounds in sediment samples. Aldehydes are rare compounds found in the surface environment, particularly in sediments. To date, aldehydes have not been used as environmental proxies. In this study, long-chain aldehydes detected from coral collected from the east coast of Kenya are analyzed by gas chromatography mass spectrometry (GC/MS) using the typical procedure for biomarker analysis. The retention time of the long-chain aldehydes and fatty acid methyl esters slightly overlapped. Hence, the peak corresponding to the aldehyde in the GC chromatogram is buried with that corresponding to the ester, possibly overlooking the aldehyde. After assessing the difference in the retention time between the aldehydes and fatty acids methyl ester, the aldehydes were easily detected using the standard analytical procedure for biomarkers analysis. A molecular ion (M+) with greater than 23 carbon atoms was detected from long-chain aldehydes. The base peak was observed at m/z 82 in the mass spectra of the aldehyde, where characteristic 68 + 14n ions corresponding to even-numbered ions were observed. The M-18 ion, which was formed by the loss of H2O, as well as M-46 or M-84 ions, was characteristic ions observed for long-chain aldehydes of the number of all carbon. The results obtained from this work, in which aldehydes were identified from coral samples, represent a good example of what could be achieved by geochemists when working with sediment samples and using aldehydes as environmental proxies.

Evaluation of the Equality of Non-Polar Capillary Columns in GC/MS Analysis of Food Contact Plastics

Non-polar capillary columns for GC/MS are widely utilized in the analysis of additives for food contact materials. Though various kinds of non-polar capillary columns are commercially available, the equality of their performance has not been verified. Herein, ninety-six additives for food contact plastics were analyzed using fifteen kinds of columns, and the peak separation, retention times, and peak areas of each additive were compared. The additives, with various chemical properties, comprised forty four plasticizers, twenty lubricants, twenty antioxidants, nine ultraviolet absorbers, and three other compounds. 10 μg.mL-1 test solutions were prepared in acetone, and injected to the GC/MS. The fifteen columns were classified into five categories based on the chromatogram pattern and peak separation. To facilitate comparison of the retention time and detection sensitivity of the columns for the additives, the relative retention time (RRT) and relative peak area (RPA) were calculated by using dibutylphthalate or 4-tert-butylphenylsalicylate as an internal standard. The RRTs of the additives on each column were essentially similar. However, the RRT of the additives which were detected in the later stages differed slightly. Although the RPA of the plasticizers and lubricants were roughly similar, column-to-column differences were observed for certain additives, such as antioxidants and ultraviolet absorbers. Furthermore, certain fatty acids, antioxidants, two plasticizers, and two benzophenone type ultraviolet absorbers were not detected in the chromatograms of two columns.

Analysis of GC×GC fingerprints from medicinal materials using a novel contour detection algorithm:A case of Curcuma wenyujin

This study introduces an innovative contour detection algorithm,PeakCET,designed for rapid and efficient analysis of natural product image fingerprints using comprehensive two-dimensional gas chromatogram(GC×GC).This method innovatively combines contour edge tracking with affinity propagation(AP)clustering for peak detection in GC×GC fingerprints,the first in this field.Contour edge tracking signif-icantly reduces false positives caused by“burr”signals,while AP clustering enhances detection accuracy in the face of false negatives.The efficacy of this approach is demonstrated using three medicinal products derived from Curcuma wenyujin.PeakCET not only performs contour detection but also employs inter-group peak matching and peak-volume percentage calculations to assess the compositional similarities and differences among various samples.Furthermore,this algorithm compares the GC×GC fingerprints of Radix/Rhizoma Curcumae Wenyujin with those of products from different botanical origins.The findings reveal that genetic and geographical factors influence the accumulation of secondary metabolites in various plant tissues.Each sample exhibits unique characteristic components alongside common ones,and vari-ations in content may influence their therapeutic effectiveness.This research establishes a foundational data-set for the quality assessment of Curcuma products and paves the way for the application of computer vision techniques in two-dimensional(2D)fingerprint analysis of GC×GC data.

基于GC-IMS和GC-MS技术结合化学计量法分析干燥方式对香椿挥发性成分的影响

为研究干燥方式对香椿挥发性风味物质的影响,利用气相色谱-离子迁移谱技术(gaschromatography-ion mobility spectrometry,GC-IMS)和气相色谱-质谱联用技术(gas chromatography-mass spectrometry,GC-MS)、相对香气活性值(relative odor activity value,ROAV)对真空冷冻干燥、热泵干燥、热风干燥、微波真空干燥的香椿样品进行挥发性成分分析,并进一步结合化学计量方法主成分分析(principal component analysis,PCA)和偏最小二乘判别分析(partial least squares-discriminant analysis,PLS-DA),探究样品间挥发性成分的差异性。结果表明,通过GC-IMS检测到78个峰,鉴定出59种化合物。通过GC-MS鉴定出94种挥发性化合物,主要挥发性成分是硫化物、烯烃类和醛类。经过干燥后总挥发性化合物的含量显著降低。通过ROAV法确定了(E,Z)-二-1-丙烯基二硫化物、2-巯基-3,4-二甲基-2,3-二氢噻吩、正己醛、2-己烯醛、丁香酚等为香椿样品中关键香气化合物。PCA和PLS-DA结果表明,不同干燥方式的样品与新鲜样品有明显的分离,彼此之间也有明显的区别。鲜样和真空冷冻干燥样品为一组,其他3个干燥香椿样品为一组。根据变量投影重要性(variable importance in projection,VIP)得分共筛选出10种(VIP>1)标志挥发性化合物。干燥方式对香椿风味特性影响显著,真空冷冻干燥组与鲜样最为接近,考虑实际应用热泵干燥为香椿最适宜的脱水方式。本研究为热加工过程中风味品质控制提供一定的理论参考。

GC-MS结合电子鼻技术对不同茶区茉莉花茶香气的差异比较

为探究不同产区茉莉花茶香气差异,采用气相色谱-质谱(GasChromatography-Mass Spectrometry,GC-MS)结合电子鼻(Electronic Nose,E-nose)技术对西南、华南、江南三大茶区的8种茉莉花茶进行香气研究。结果表明,8个样品共鉴定出香气成分58种,其中西南、江南、华南茶区分别为45种、51种、47种。江南茶区香气化合物总量最高。共有香气成分主要包括邻氨基苯甲酸甲酯、顺式-3-己烯醇苯甲酸酯、乙酸苄酯、水杨酸甲酯、芳樟醇、吲哚等。其中水杨酸甲酯在江南茶区含量最高(22.32μg/g),分别较华南、西南茶区高33.96%、68.01%;邻氨基苯甲酸甲酯(67.39μg/g)和吲哚(43.84μg/g)含量在华南茶区最高。茉莉花茶香气评价指数(JasmineTea Flavor Index,JTF index)分析表明西南茶区样品等级最高。香气聚类分析将共有香气成分分为3类,分别呈花香、茉莉花香和草木香。通过电子鼻技术可知样品香气物质变化与硫化物、碳氢化合物、芳香化合物有关,并能有效区别样品香气。综上,三大茶区样品香气种类差异不明显,但各香气成分含量差异显著(P<0.05),江南和华南茶区的样品特征性香气成分含量较高,西南茶区样品综合指数高。

SPME-HS-GC-MS与电子鼻分析不同产地多花酒黄精气味特征

目的:分析不同产地多花酒黄精的气味特征,为产地判别、分析方法改进提供依据。方法:以11个产地的多花酒黄精细粉为研究样品,采用固相微萃取-顶空进样-气质联用法(SPME-HS-GC-MS)分析多花酒黄精挥发性成分,采用电子鼻智能感官评定技术分析多花酒黄精气味雷达图,采用主成分(PCA)、Loadings方法分析电子鼻信号响应结果,构建产地判别模型。结果:SPME-HS-GC-MS法结果共鉴别出32个挥发性成分,其中19个差异性挥发性成分可用于8个产地的区分。电子鼻结果表明,主成分判别分析能较好地区分不同产地多花酒黄精,多花酒黄精在气味上的差异主要体现在芳香成分,氮氧化合物、氨类、烷烃、甲烷等短链烷烃、无机硫化物、有机硫化物等。结论:不同产地多花酒黄精的气味特征存在差异,可作为产地判别依据。电子鼻技术可为多花酒黄精分析及质量标准提供简单、快速的新方法。

硅烷衍生化GC-MS检测香精中糖类物质成分

建立了基于硅烷衍生化气相色谱-质谱联用法快速检测香精中17种糖类物质的方法。结果表明:衍生化的最佳条件为以BSTFA为衍生化试剂、衍生化温度40℃、衍生化时间40 min,在此条件下共鉴定出17种糖类物质。17种糖类物质在一定质量浓度内具有良好的线性关系(R^(2)>0.99)。方法的检出限为0.027~0.077μg/mL,加标回收率为94.80%~110.03%,相对标准偏差为3.03%~8.06%。实际样品测定结果表明,建立的方法能够快速准确地检测香精中17种糖类物质成分,满足对香精中糖类物质的同时检测。

HS-GC-MS联用测定河南传统西瓜豆酱中的挥发性成分

以河南传统发酵的西瓜豆酱为研究对象,采用自动顶空进样-气质联用(HS-GC-MS)法测定其挥发性成分。通过单因素试验分别考察了平衡温度、平衡时间、震动频率及样品氯化钠的添加量对挥发性成分的影响。结果表明,平衡温度90℃,平衡时间50 min,震动频率6次/秒,不添加氯化钠为测定较优条件。在此条件下,鉴定出自然发酵西瓜豆酱中挥发性成分有10类共82种,其中醇类12种,酯类10种,烯烃类14种,醛类6种,酮类8种,醚类4种,酸类1种,烷烃类10,含N化合物7种和其他10种。相对含量较高的是烯烃类、醛类和醇类,分别为23.848%,22.537%和19.743%,三者之和占挥发性成分总量的66.12%,其次是酯类和酮类,分别占11.945%和6.839%,这三种成分对河南传统西瓜豆酱的特征风味起着至关重要的作用。

不同厂家水基胶挥发性物质的GC-IMS差异分析

目的快速分析不同厂家水基胶中的挥发物特性。方法采用气相色谱-离子迁移谱(GC-IMS)联用技术对各种水基胶中的挥发性物质进行定性分析;结合生物指纹图谱、主成分分析(PCA)法以及欧式距离分析法对不同水基胶样品进行差异对比分析。结果水基胶中共识别出88种挥发性化学物质,涵盖酯类、酮类、醇类、醛类、杂环类、酸类、芳香类、醚类、萜类、酰胺类和腈类等11大类别,其中酯类物质占据显著比例,达26种,占总挥发性物质的38%~46%。结论采用GC-IMS技术结合生物指纹图谱、PCA以及欧式距离分析,能够有效区分不同厂家水基胶样品,同时同一厂家不同规格样品之间显示出较高的相似性;GC-IMS技术为不同厂家水基胶的快速溯源鉴别及挥发性物质差异分析提供了有力工具。

SPE-GC-FPD法测定三七中甲基对硫磷残留量

目的:为更好地控制三七质量,拟建立三七中甲基对硫磷的GC-FPD检测方法。方法:采用超声提取固相萃取法、GC-FPD检测。结果:方法回收率在62.52%~118.49%,精密度RSD为3.597%,标准偏差符合检测要求,满足农药残留检测的要求。

基于GCS评分的Nomogram图预测急性脑出血后卒中相关性肺炎的发生风险

目的 通过构建Nomogram预测模型,探讨急性脑出血后发生卒中相关性肺炎(SAP)的危险因素。方法 回顾性分析2018-01—2022-12平顶山学院第一附属医院神经外科、重症医学科及神经重症的1 050例急性脑出血患者的临床资料,先根据GCS评分进行感染率的分层分析,然后运用组间差异性比较及多因素Logistic回归分析筛选SAP的独立危险因素,应用R语言构建Nomogram预测模型,并对构建的模型进行评价。结果 急性脑出血患者中SAP发生率为35.9%,其中GCS评分3~8分患者为77.21%,GCS评分9~12分患者为30.81%,GCS评分13~15分患者为6.50%,各组间感染率差异有统计学意义(P<0.05)。多因素Logistic回归显示,年龄、GCS评分、入院时随机血糖、淋巴细胞绝对值及手术治疗均为SAP独立危险因素,以这5个危险因素构建的Nomogram预测模型可帮助临床医师预测急性脑出血后SAP发生风险,具有较高的准确性和临床适用性。结论 基于GCS评分构建的Nomogram预测模型能够在疾病早期阶段准确高效地对急性脑出血患者发生SAP的风险进行分层,识别出易发生SAP患者的高风险人群,从而采取有针对性的干预措施。

闽南产罗勒不同部位挥发油的GC-MS成分分析及其抑菌活性比较

目的对闽南产罗勒不同部位挥发油的成分进行分析及抑菌活性比较。方法通过水蒸气蒸馏法提取闽南产罗勒不同部位(种子、叶、根、茎)的挥发油,采用气相色谱-质谱(GC-MS)联用技术,鉴定其化学成分组成;并以金黄色葡萄球菌和大肠杆菌作为鉴定菌,采用滤纸片扩散法比较罗勒四个部位挥发油的体外抗菌活性。结果从闽南产罗勒种子、叶、根、茎分别鉴定出30、26、16和26种挥发性化合物;种子和叶片的抑菌活力显著,根部和茎部的抑菌活性弱。结论罗勒种子和叶子在化学成分种类和主成分含量上相近,并表现出对金黄色葡萄球菌和大肠杆菌相当的抑菌活性;根、茎部挥发油的抑菌力弱。

基于GC-MS和快速气相电子鼻对我国东北地区代表性粳米香气组分分析

为探究我国东北地区4种代表性粳米(香米五优稻4号、绥粳18和非香米龙粳31、盐丰47)香气组分差异,通过顶空-固相微萃取-气相色谱-质谱联用(HS-SPME-GC-MS)和快速气相电子鼻(Flash GC e-nose)技术对粳米香气组分进行鉴定。研究采用正交偏最小二乘法-判别分析(OPLS-DA)和层次聚类分析(HCA)等方法对4种粳米香气组分进行分析,结果表明,4种粳米的主要香气组分构成类似,以己醛、壬醛等醛类为主;五优稻4号主要香气成分含量显著(P≤0.05)高于其他3个品种粳米,使得其香气更加浓郁;关于粳米香气组分鉴定技术,GC-MS技术的准确度和检测范围优于电子鼻技术,而检测效率低于电子鼻技术。

托里阿魏挥发油的GC-MS指纹图谱及抗宫颈癌作用研究

目的建立托里阿魏挥发油的气相色谱-质谱(GC-MS)指纹图谱,并考察托里阿魏挥发油的抗宫颈癌作用。方法采用有机溶剂提取法提取托里阿魏根的挥发油,并通过GC-MS鉴定所含成分。通过MTT比色法考察不同浓度托里阿魏挥发油对人宫颈癌Hela细胞增殖的抑制作用。采用Transwell法检测托里阿魏挥发油对人宫颈癌Hela细胞迁移、侵袭能力的影响。应用流式细胞术检测托里阿魏挥发油作用下的细胞凋亡率。结果托里阿魏挥发油中鉴别出58种化学成分,含量最多的是孕酮。托里阿魏挥发油对人宫颈癌Hela细胞的增殖有一定的抑制作用,IC50为55.21μg/ml。托里阿魏高、低剂量组与对照组相比,迁移和侵袭细胞数量显著减少(P<0.01)。结论托里阿魏挥发油中含量最高的是酮类化合物。托里阿魏提取物有一定的抗肿瘤作用。

快速高效区分黄檀属黑酸枝木的方法-GC/MS指纹图谱

采用气相色谱-质谱指纹图谱分别鉴定阔叶黄檀、卢氏黑黄檀、东非黑黄檀和伯利兹黄檀木材。以二氯甲烷提取样品中的特定化合物,采用气相色谱-质谱法分析提取物,建立目标物色谱图。采用二氯甲烷溶剂提取阔叶黄檀、卢氏黑黄檀、东非黑黄檀和伯利兹黄檀4种黄檀属黑酸枝木,其提取液用气相色谱质谱联用仪分析,结果显示该4种树种的特征色谱峰不同。阔叶黄檀的色谱峰在14.6min、14.8min出现双子色谱峰,强度相似;卢氏黑黄檀分别在11.9min、12.5min、12.9min有3个强度相似的色谱峰;东非黑黄檀的强度大的特征峰在18.3min和18.5min;伯利兹黄檀仅有1个强度大的色谱峰,其保留时间在17.1min。分析这4种木材的GC/MS指纹图谱,色谱峰的保留时间不同。该方法可以有效区分鉴别这4种黑酸枝木。

GC-MS分析大莪术根茎挥发油成分

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