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Liquid-solid mass transfer in a rotating packed bed reactor with structured foam packing 被引量:2
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作者 Yazhao Liu Zhi hao Li +3 位作者 Guangwen Chu Lei Shao Yong Luo Jianfeng Chen 《Chinese Journal of Chemical Engineering》 SCIE EI CAS CSCD 2020年第10期2507-2512,共6页
A rotating packed bed(RPB) reactor has substantially potential for the process intensification of heterogeneous catalytic reactions. However, the scarce knowledge of the liquid–solid mass transfer in the RPB reactor ... A rotating packed bed(RPB) reactor has substantially potential for the process intensification of heterogeneous catalytic reactions. However, the scarce knowledge of the liquid–solid mass transfer in the RPB reactor is a barrier for its design and scale-up. In this work, the liquid–solid mass transfer in a RPB reactor installed with structured foam packing was experimentally studied using copper dissolution by potassium dichromate. Effects of rotational speed, liquid and gas volumetric flow rate on the liquid–solid mass transfer coefficient(kLS) have been investigated. The correlation for predicting kLSwas proposed, and the deviation between the experimental and predicted values was within±12%. The liquid–solid volumetric mass transfer coefficient(kLSaLS) ranged from 0.04–0.14 1^-1, which was approximately 5 times larger than that in the packed bed reactor. This work lays the foundation for modeling of the RPB reactor packed with structured foam packing for heterogeneous catalytic reaction. 展开更多
关键词 Rotating packed bed Liquid–solid mass transfer Structured foam packing Process intensification
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Evaluation of Sensitivity and Positive Predictive Values of Cytopathologic Diagnosis of Solid Masses in Dogs
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作者 Richard M. Kabuusu Tracy Volger +7 位作者 Sachin Kumthekar Keshaw Tiwari Alfred Chikweto Muhammad I. Bhaiyat Claude De Allie Ruth Alexander Carla Richards Ravindra N. Sharma 《Open Journal of Veterinary Medicine》 2016年第6期95-98,共4页
In this retrospective study, a total of 275 solid masses were examined for cytopathologic diagnosis. Twenty four percent (67/275) of these cytologic samples were followed by surgical biopsy and histopathologic diagnos... In this retrospective study, a total of 275 solid masses were examined for cytopathologic diagnosis. Twenty four percent (67/275) of these cytologic samples were followed by surgical biopsy and histopathologic diagnosis, allowing for comparisons. On average, the cutaneous and subcutaneous solid masses were recognized when the dogs were aged between 6 and 9 years old. The origins of the solid masses included connective tissue tumors 37.1% (23/62), epithelial tissue tumors 33.9% (21/62), round cell tumors 19.4% (12/62), masses of inflammatory lesions 4.8% (3/62) and lesions due to other causes 4.8% (3/62). The sensitivity and positive predictive value (PPV) of cytopathology in the diagnosis of solid masses were 93% (62/67) and 97% (62/64), respectively. Generally, neo-plasms were over diagnosed by cytopathology as was indicated by the positive predictive value. Both the sensitivity and the PPV of cytopathology comparative to histopathology in the diagnosis of inflammatory processes were 100% (3/3). The inflammatory lesions were eventually confirmed as necrotizing myositis, necro-suppurative cystitis and endocrine inflammatory dermatopathy based on histopathology. Less than 8% (5/67) of samples were incorrectly diagnosed by cytology. The study showed high accuracy between cytological and histopathological examination of solid masses in dogs, and thus a reliable diagnostic tool in patient care. 展开更多
关键词 CYTOPATHOLOGY HISTOPATHOLOGY DOG Sensitivity Positive Predictive Value solid masses
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Prediction of Core-Annulus Solids Mass Transfer Coefficient in Gas-Solid Fluidized Bed Risers
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作者 刘新华 高士秋 宋文立 《Chinese Journal of Chemical Engineering》 SCIE EI CAS CSCD 2005年第5期577-582,共6页
Based on analysis of energy dissipation in the core region of gas-solid fluidized bed risers, a simplified model for determination of core-annulus solids mass transfer coefficient was developed according to turbulent ... Based on analysis of energy dissipation in the core region of gas-solid fluidized bed risers, a simplified model for determination of core-annulus solids mass transfer coefficient was developed according to turbulent diffusion mechanism of particles. The simulation results are consistent with published experimental data. Core-annulus solids mass transfer coefficient decreases with increasing particle size, particle density and solids circulation rate,but generally increases with increasing superficial gas velocity and riser diameter. In the upper dilute region of gas-solid fluidized bed risers, core-annulus solids mass transfer coefficient was found to change little with the axial coordinate in the bed. 展开更多
关键词 solids mass transfer coefficient core-annulus structure turbulent diffusion gas-solid fluidization
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Simultaneous Determination of Bisphenols and Alkylphenols in Water by Solid Phase Extraction and Ultra Performance Liquid Chromatography-tandem Mass Spectrometry 被引量:4
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作者 SHAN Xiao Mei SHEN Deng Hui +2 位作者 WANG Bing Shuang LU Bei Bei HUANG Fa Yuan 《Biomedical and Environmental Sciences》 SCIE CAS CSCD 2014年第6期471-474,共4页
To establish an analytical method for determination of four bisphenols (BPA, BPB, BPF, and BPS) and two alkylphenols (4-n-OP, 4-n-NP) in water by ultra performance liquid chromatography- tandem mass spectrometry ... To establish an analytical method for determination of four bisphenols (BPA, BPB, BPF, and BPS) and two alkylphenols (4-n-OP, 4-n-NP) in water by ultra performance liquid chromatography- tandem mass spectrometry (UPLC/MS/MS). The water samples were extracted and condensed with solid-phase extraction (SPE) using C18 cartridges and eluted by acetonitrile. Separation was carried out with Acquity BEH C8 column and detection were performed by UPLC/MS/MS. Quantification was calculated by using the internal standard BPA-d16 and 4-n-NP-d8. The linear correlation coefficients of these compounds in the range of 1.0-100.0μg/L were all over 0.999. The minimum detectable concentrations were 0.75-1.0 ng/L, and the recoveries ranged from 87.0% to 106.9%. 展开更多
关键词 UPLC BPA Simultaneous Determination of Bisphenols and Alkylphenols in Water by solid Phase Extraction and Ultra Performance Liquid Chromatography-tandem mass Spectrometry mass
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MASS TRANSPORT IN SOLID TUMORS(Ⅱ)──DRUG DELIVERY
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作者 雷晓晓 吴望一 +1 位作者 温功碧 陈建国 《Applied Mathematics and Mechanics(English Edition)》 SCIE EI 1998年第12期0-0,0-0+0-0+0-0+0-0,共10页
关键词 CI DRUG DELIVERY mass TRANSPORT IN solid TUMORS
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Design of fan beam optical sensor and its application in mass flow rate measurement of pneumatically conveyed solids
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作者 李扬 郑莹娜 岳洪伟 《Journal of Zhejiang University-Science A(Applied Physics & Engineering)》 SCIE EI CAS CSCD 2005年第12期1430-1434,共5页
The fan-beam optical sensor is made up of many semiconductor lasers and detectors fixed around the wall alternately at a cross section of pneumatically conveying pipe. When the sensor works, a scanning light source em... The fan-beam optical sensor is made up of many semiconductor lasers and detectors fixed around the wall alternately at a cross section of pneumatically conveying pipe. When the sensor works, a scanning light source emits a 50° lamellar fan-beam through the gas-solid two phase flow, and the projection data resulting extinction effect of solid particles are detected at the same time. With the projection data, the flow rate mass can be calculated, and then the flow image can be reconstructed. In this paper, the design of the sensor including spatial arrangement of the structural parts, basic principle and measurement sensitivity distribution are introduced. The mathematical measurement model of solid mass flow rate is presented together with the testing results. 展开更多
关键词 Optical sensor Fan-beam laser Pneumatic conveyor system mass flow rate of solids
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Multiresidue Method for Determination of 67 Pesticides in Water Samples Using Solid-Phase Extraction with Centrifugation and Gas Chromatography-Mass Spectrometry 被引量:3
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作者 Abir Kouzayha Abdul Rahman Rabaa +3 位作者 Mohamad Al Iskandarani Daniel Beh Hélène Budzinski Farouk Jaber 《American Journal of Analytical Chemistry》 2012年第3期257-265,共9页
A new multi-residue method based on solid-phase extraction (SPE) with centrifugation was developed for determination and quantitation of 67 pesticides in water samples. Two SPE cartridges were tested: Chromabond C18 a... A new multi-residue method based on solid-phase extraction (SPE) with centrifugation was developed for determination and quantitation of 67 pesticides in water samples. Two SPE cartridges were tested: Chromabond C18 and Oasis HLB. Parameters that influence the extraction efficiency such as the eluent volume, the sample loading volume, the addition of organic solvent to water sample, sorbent drying and elute concentration were optimized. The innovation of this work was the examination of the use of a centrifugation technique in both the drying and elution steps. When combined with centrifugation, the volume of the elution solvent was reduced to 2 mL and the time for sorbent drying decreased also to 10 min under vacuum. Under the optimized conditions, this method showed good recoveries higher than 65% - 68% for the 67 analyzed pesticides using the C18 and HLB cartridges with relative standard deviations lower than 9.7% - 12.3%. Limits of quantification were between 2 and 20 ng.L–1. The simplicity of the described method, use of less of organic solvent, short procedure time, and good recoveries demonstrate the advantages of this environmentally friendly approach for routine analysis of numerous samples. 展开更多
关键词 MULTI-RESIDUE PESTICIDES solid-PHASE Extraction CENTRIFUGATION Gas Chromatography-mass SPECTROMETRY
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Uncertainty Evaluation of Determination of Microcystin MC-LR in Environmental Samples by Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry 被引量:1
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作者 Zhao Bin Zhang Min Zhang Fuhai 《Meteorological and Environmental Research》 CAS 2016年第6期54-57,共4页
To assess uncertainty of determination of MC-LR in environmental samples by solid phase extraction- ultra performance liquid chromatography- tandem mass spectrometry,the sources of the uncertainty were evaluated first... To assess uncertainty of determination of MC-LR in environmental samples by solid phase extraction- ultra performance liquid chromatography- tandem mass spectrometry,the sources of the uncertainty were evaluated firstly,and the expanded uncertainty was calculated finally.The results show that when MC-LR concentration in the water samples was 0.50 μg/L,the expanded uncertainty was 0.00628 μg/L(k=2). 展开更多
关键词 Uncertainty solid phase extraction Ultra performance liquid CHROMATOGRAPHY TANDEM mass SPECTROMETRY MICROCYSTIN MC-LR China
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Improved preparation and identification of aristolochic acid-DNA adducts by solid-phase extraction with liquid chromatography-tandem mass spectrometry
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作者 GAO Haiyan GUO Fangqiu +3 位作者 FENG Feng YIN Junfa SONG Maoyong WANG Hailin 《Journal of Environmental Sciences》 SCIE EI CAS CSCD 2009年第12期1769-1776,共8页
Aristolochic acid (AA) is a known nephrotoxin and potential carcinogen, which can form covalent DNA adducts after metabolic activation in vivo and in vitro. A simple method for preparation and characterization of ar... Aristolochic acid (AA) is a known nephrotoxin and potential carcinogen, which can form covalent DNA adducts after metabolic activation in vivo and in vitro. A simple method for preparation and characterization of aristolochic acid-DNA adducts was developed. Four AA-adducts were synthesized by a direct reaction of AAI/AAII with 2′-deoxynucleosides. The reaction mixture was first cleaned-up and pre-concentrated using solid phase extraction (SPE), and further purified by a reversed-phase high performance liquid chromatography (HPLC). By the application of developed SPE procedure, matrices and byproducts in reaction mixture could be greatly reduced and adducts of high purity (more than 94% as indicated by HPLC) were obtained. The purified AA-DNA adducts were identified and characterized with liquid-electrospray ionization-quadrupole-time of flight-mass spectrometry (LC-ESI-Q-TOF-MS/MS) and LC-Diode array detector-fluorescence (LC-DAD-FL) analysis. This work provides a robust tool for possible large-scale preparation of AA-DNA adduct standards, which can promote the further studies on carcinogenic and mutagenic mechanism of aristolochic acids. 展开更多
关键词 aristolochic acid DNA adducts solid phase extraction QUADRUPOLE time-of-flight tandem mass spectrometry
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基于HS-GC-IMS和HS-SPME-GC-MS的蛋白酶对豆粕挥发性风味的影响分析 被引量:1
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作者 齐宝坤 刘雨雯 +3 位作者 姚玉雪 吴思雨 孙树坤 陈昊 《农业机械学报》 EI CAS CSCD 北大核心 2024年第4期352-367,410,共17页
为研究不同蛋白酶酶解对豆粕挥发性风味成分的影响,选用4种蛋白酶(碱性蛋白酶、中性蛋白酶、木瓜蛋白酶、风味蛋白酶)对豆粕进行酶解,采用顶空-气相色谱-离子迁移谱(Headspace-gas chromatography-ion mobility spectroscopy,HS-GC-IMS... 为研究不同蛋白酶酶解对豆粕挥发性风味成分的影响,选用4种蛋白酶(碱性蛋白酶、中性蛋白酶、木瓜蛋白酶、风味蛋白酶)对豆粕进行酶解,采用顶空-气相色谱-离子迁移谱(Headspace-gas chromatography-ion mobility spectroscopy,HS-GC-IMS)和顶空固相微萃取-气相色谱-质谱(Headspace solid phase microextraction-gas chromatography-mass spectrometry,HS-SPME-GC-MS)联用技术分析不同豆粕酶解物(Soybean meal hydrolysates,SMH)的挥发性风味成分,并结合主成分分析(Principal component analysis,PCA)、热图聚类和正交偏最小二乘判别法(Orthogonal partial least squares-discriminant analysis,OPLS-DA)对不同SMH进行分析。结果表明:碱性蛋白酶、中性蛋白酶、木瓜蛋白酶和风味蛋白酶酶解豆粕的挥发性风味成分存在较大差异。HS-GC-IMS鉴定出84种挥发性成分,筛选得到33种差异风味物质,发现酶解后酮类物质显著降低而醛类、醇类和酯类物质含量明显增加。PCA结果表明不同SMH之间的风味存在显著差异。最终通过OPLS-DA筛选出贡献较大的挥发性化合物,同时构建出可靠的用以鉴别SMH的模型。HS-SPME-GC-MS检测出103种差异风味物质,可用于区分不同SMH,被检出的挥发性组分中醛类、醇类和酮类等化合物为SMH风味的形成做出主要贡献,明晰了部分风味化合物形成的原因。PCA和聚类热图结果表明不同蛋白酶酶解对豆粕的挥发性风味物质的种类和含量有显著影响,其中,风味蛋白酶和木瓜蛋白酶对豆粕的风味改善最为显著。 展开更多
关键词 豆粕 酶解 顶空-气相色谱-离子迁移谱 顶空固相微萃取-气相色谱-质谱
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基于HS-SPME-GC-MS的不同成熟度‘青皮’无花果挥发性成分分析
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作者 刘雪梅 闫新焕 +4 位作者 谭梦男 谷思梦 杜文瑜 许敏 宋烨 《中国果菜》 2024年第4期14-19,共6页
为探讨不同成熟度威海‘青皮’无花果挥发性成分差异,本研究采用固相微萃取(SPME)和气相色谱-质谱联用技术(GC-MS)对鲜食无花果挥发性成分进行分析,并采用内标法对风味物质进行定量分析。结果显示,在威海‘青皮’无花果中共检测出73种... 为探讨不同成熟度威海‘青皮’无花果挥发性成分差异,本研究采用固相微萃取(SPME)和气相色谱-质谱联用技术(GC-MS)对鲜食无花果挥发性成分进行分析,并采用内标法对风味物质进行定量分析。结果显示,在威海‘青皮’无花果中共检测出73种挥发性成分,主要为酯类、醛类、醇类、烯类、烷烃类等,其中六成熟无花果检出33种、八成熟检出29种、十成熟检出36种。不同成熟度无花果的挥发性组分、特征风味物质种类和含量差异明显。 展开更多
关键词 无花果 挥发性成分 气相色谱-质谱联用技术 固相微萃取
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贵州不同芒果品种(系)果实香气成分研究
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作者 刘清国 刘荣 +4 位作者 黄海 张正学 林迓 党志国 雷跃 《贵州农业科学》 CAS 2024年第11期92-101,共10页
【目的】测定贵州不同芒果品种(系)的香气成分及其相对含量,明确其香气特性,为选育优质芒果新品种提供参考。【方法】以金煌芒、台农1号芒和台芽芒等32个芒果品种(系)为试验材料,采用顶空固相微萃取-气质联用技术测定分析不同品种(系)... 【目的】测定贵州不同芒果品种(系)的香气成分及其相对含量,明确其香气特性,为选育优质芒果新品种提供参考。【方法】以金煌芒、台农1号芒和台芽芒等32个芒果品种(系)为试验材料,采用顶空固相微萃取-气质联用技术测定分析不同品种(系)的香气成分类别及其相对含量,明确其香气特性。【结果】金煌芒、台农1号芒和台芽芒等32个芒果品种(系)共检测出9类103种香气成分,依次为倍半萜烯类(25种)>单萜烯类(21种)>酯类(14种)>醇类(11种)>醛类=其他物质(10种)>酮类(8种)>酸类(3种)>芳香烃类(1种);以月桂烯、3-蒈烯、γ-松油烯、(E,E)-4,6-二甲基-2,4,6-辛三烯和反式石竹烯为芒果香气的基本组成成分。台芽芒的香气种类最多,为54种;椰香芒最少,仅28种。果实的醇类和酯类物质较少,且相对含量均小于10.00%。32个芒果品种(系)聚为2类,类群1包括生吃芒、桂七芒、爱文芒、鹰嘴芒和桂热10号芒;类群2分为2个分支,第一分支包括台牙芒、贵妃芒、QS-002、金兴芒、玉文芒、东镇红芒、热品2号芒、热农1号芒、红芒6号、黔山芒1号和凯特芒,其余16个芒果品种(系)归为第二分支。【结论】贵州不同芒果品种(系)果实的香气成分丰富,共检测出9类103种香气成分,其相对含量存在明显差异,以月桂烯、3-蒈烯、γ-松油烯、(E,E)-4,6-二甲基-2,4,6-辛三烯和反式石竹烯为芒果香气的基本组成成分。 展开更多
关键词 芒果 品种(系) 香气特性 顶空固相微萃取法 气相色谱-质谱分析 贵州
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固相萃取-液相色谱-串联质谱法测定海参中62种兽药残留
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作者 汤水粉 钱卓真 +5 位作者 周佳敏 王丽娟 刘海新 罗方方 位绍红 陈燕婷 《食品安全质量检测学报》 CAS 2024年第12期230-239,共10页
目的建立固相萃取结合高效液相色谱-串联质谱同时测定海参中62种药物的检测方法。方法样品加水分散后经1.0%甲酸乙腈溶液提取,PEP固相萃取柱净化后,采用WatersX-Bridge-C18色谱柱分离、0.2%甲酸水溶液-甲醇为流动相进行梯度洗脱,使用选... 目的建立固相萃取结合高效液相色谱-串联质谱同时测定海参中62种药物的检测方法。方法样品加水分散后经1.0%甲酸乙腈溶液提取,PEP固相萃取柱净化后,采用WatersX-Bridge-C18色谱柱分离、0.2%甲酸水溶液-甲醇为流动相进行梯度洗脱,使用选择离子监测模式检测。结果62种兽药在0.50~100.00ng/m L范围内呈现出良好的线性关系,线性相关系数r^(2)在0.9953~1.0000范围内。方法检出限为0.25~2.50μg/kg;在3个不同浓度添加水平下,62种兽药的平均回收率在70.3%~119.0%,批内和批间的相对标准偏差(n=5)为0.13%~14.90%,均小于15.00%。将该方法应用于30批次海参样品的检测,其中4批次样品的喹诺酮检测结果阳性,检出量为5.30~28.00μg/kg,与国家标准方法的检测结果相比,该方法对于本次喹诺酮药物筛查的准确率为100%。结论该方法灵敏度高,准确度和精密度良好,满足我国兽药残留检测要求,可适用于海参中62种兽药多残留的定性定量分析检测。 展开更多
关键词 固相萃取 高效液相色谱-串联质谱法 海参 兽药残留
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固相萃取结合液质联用法快速筛查和分析生活饮用水中的56种抗生素
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作者 陈琨 钟格梅 +3 位作者 韦日荣 黄江平 雷宁生 廖艳华 《食品安全导刊》 2024年第13期39-46,50,共9页
目的:建立生活饮用中56种抗生素的固相萃取-液相色谱-串联质谱分析方法。方法:将生活饮用水通过大容量采样管连接到固相萃取柱上净化,用C18柱梯度洗脱分离目标物,以乙腈和0.1%甲酸水为流动相,经电喷雾离子源电离,多反应监测模式串联质... 目的:建立生活饮用中56种抗生素的固相萃取-液相色谱-串联质谱分析方法。方法:将生活饮用水通过大容量采样管连接到固相萃取柱上净化,用C18柱梯度洗脱分离目标物,以乙腈和0.1%甲酸水为流动相,经电喷雾离子源电离,多反应监测模式串联质谱检测。结果:56种抗生素的最低检测浓度为0.1~2.0μg·L^(-1),在其线性范围内的相关系数均大于0.995,3个浓度水平的加标回收率为63.3%~113.0%,相对标准偏差在3.1%~8.3%。结论:该方法前处理简单、快速,适用于生活饮用水中多种抗生素的快速筛查和定量检测。 展开更多
关键词 超高效液相色谱-串联质谱 固相萃取 生活饮用水 大容量采样管
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不同产地沃柑挥发性成分的差异分析 被引量:1
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作者 张耀海 陈细羽 +1 位作者 王成秋 焦必宁 《食品与发酵工业》 CAS CSCD 北大核心 2024年第5期297-304,共8页
该研究旨在分析4个主产地(四川、重庆、云南和广西)的沃柑果皮中挥发性成分的差异性,并为沃柑的产地溯源和深加工提供数据支撑。利用顶空固相微萃取-气相色谱-质谱联用技术测定了沃柑果皮挥发性成分,共鉴定出50种挥发性成分,其中萜烯类1... 该研究旨在分析4个主产地(四川、重庆、云南和广西)的沃柑果皮中挥发性成分的差异性,并为沃柑的产地溯源和深加工提供数据支撑。利用顶空固相微萃取-气相色谱-质谱联用技术测定了沃柑果皮挥发性成分,共鉴定出50种挥发性成分,其中萜烯类18种、醇类11种、醛类10种、酯类8种、酮类1种、其他类2种。柠檬烯是主要的挥发性物质,月桂烯、α-蒎烯、芳樟醇、正辛醇、正辛醛、香茅醇、己醛、反式-2-己烯醛、桧烯、香芹酮和α-松油醇等次之。基于挥发性成分半定量结果,建立四川和重庆,云南和广西沃柑的正交偏最小二乘法判别分析模型,进而筛选出潜在生物标志物。结果表明,柠檬烯、芳樟醇和香茅醇可作为区分重庆和四川的潜在生物标志物,醋酸辛酯和α-松油醇可作为区分广西和云南的潜在生物标志物。 展开更多
关键词 沃柑 挥发性成分 顶空固相微萃取 气相色谱-质谱联用
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基于多元统计学分析^(60)Co-γ射线辐照对川芎挥发性成分的影响
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作者 王艳 孟爱莲 +7 位作者 贾鑫 叶嘉伟 徐攀 张雁君 邱娅璐 何江 毛腾霄 高鹏 《辐射研究与辐射工艺学报》 CAS CSCD 2024年第4期75-88,共14页
川芎挥发性成分是其主要活性成分之一,也是评价川芎药用品质的重要指标。为探究^(60)Co-γ射线辐照对川芎挥发性成分的影响,本研究以不同吸收剂量处理川芎样品,采用电子鼻结合顶空固相微萃取-气相色谱-质谱技术(HS-SPME-GC-MS),通过主... 川芎挥发性成分是其主要活性成分之一,也是评价川芎药用品质的重要指标。为探究^(60)Co-γ射线辐照对川芎挥发性成分的影响,本研究以不同吸收剂量处理川芎样品,采用电子鼻结合顶空固相微萃取-气相色谱-质谱技术(HS-SPME-GC-MS),通过主成分分析、线性判别分析、正交偏最小二乘法和聚类分析的多元统计学方法分析数据,以期了解川芎辐照前后挥发性成分的变化。电子鼻与GC-MS结果都表明:川芎气味主要由烷烃类、醇类、醛类、酮类贡献,10 kGy剂量以下的辐照处理对川芎挥发性气味成分影响不大;川芎经0 kGy(对照组)、3 kGy、7 kGy、10 kGy剂量辐照处理后,共鉴定出60种化合物,其中烃类23种,醇类12种,脂类10种,醛酮类4种,其他类11种;筛选到21种辐照前后的差异特征性指标物,它们在川芎挥发性成分中只占约12.92%,不是川芎的主要挥发性成分。经10 kGy剂量以下的辐照处理后,川芎中没有新生成的物质被鉴定出来。研究结果提示经10 kGy以下剂量处理川芎不会影响其主要挥发性成分。 展开更多
关键词 川芎 辐照 挥发性成分 顶空固相微萃取-气相色谱-质谱技术 多元统计学分析
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固相萃取结合高效液相色谱-串联质谱测定胎便中14种全氟和多氟烷基化合物 被引量:1
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作者 刘超 何安恩 +2 位作者 罗雅丹 黎娟 王亚韡 《环境化学》 CAS CSCD 北大核心 2024年第5期1553-1564,共12页
全氟和多氟烷基化合物(PFASs)是一类人工合成的物质,由于其热稳定、疏水、疏油等优良性质而被广泛使用于生活和生产中.PFASs具有环境持久性、生物累积性、多种毒性等特性,且可以通过胎盘屏障进入到胎儿体内,进而对胎儿健康产生潜在危害... 全氟和多氟烷基化合物(PFASs)是一类人工合成的物质,由于其热稳定、疏水、疏油等优良性质而被广泛使用于生活和生产中.PFASs具有环境持久性、生物累积性、多种毒性等特性,且可以通过胎盘屏障进入到胎儿体内,进而对胎儿健康产生潜在危害.胎便中积累了妊娠期间暴露于胎儿的外源性化合物,可用于监测PFASs对胎儿的宫内暴露特征.本研究基于固相萃取结合高效液相色谱-串联质谱技术,建立了胎便中14种PFASs的分析方法.采用乙腈/水(9∶1,V/V)对0.2 g冻干胎便样品进行超声提取,提取液经Envi-carb和Oasis WAX小柱固相萃取,0.1%氨甲醇洗脱.以10 mmol·L^(−1)乙酸铵水溶液和乙腈作为流动相对目标化合物进行梯度洗脱,采用Acquity UPLC BEH C18色谱柱进行分离,基于多反应监测负离子模式采集,内标法定量.结果表明,在2、5、20 ng·g^(−1)的加标浓度下,14种PFASs的回收率为65%—149%,相对标准偏差为3%—22%,方法检出限(MDLs)为0.001—0.149 ng·g^(−1),方法定量限(MQLs)为0.003—0.495 ng·g^(−1).使用该方法测定了10个胎便样品,ΣPFASs浓度范围为<MDLs—2.49 ng·g^(−1).该方法操作简单、便捷、灵敏度高且定量准确,为系统性研究胎便中PFASs的赋存特征及暴露风险提供了技术基础. 展开更多
关键词 胎便 全氟和多氟烷基化合物 高效液相色谱-串联质谱 固相萃取
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顶空箭形固相微萃取–气相色谱质谱法分析烃源岩和稠油中的金刚烷类化合物
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作者 田彦宽 詹兆文 《地球化学》 CAS CSCD 北大核心 2024年第3期399-408,共10页
采用顶空箭型固相微萃取–气相色谱质谱联用技术(HS-SPME Arrow-GC/MS)直接检测分析烃源岩粉末样品和稠油中的单金刚烷类和双金刚烷类化合物,考察并优化了影响萃取效率的萃取纤维头类型、萃取温度、萃取时间和解析时间等关键因素。对于... 采用顶空箭型固相微萃取–气相色谱质谱联用技术(HS-SPME Arrow-GC/MS)直接检测分析烃源岩粉末样品和稠油中的单金刚烷类和双金刚烷类化合物,考察并优化了影响萃取效率的萃取纤维头类型、萃取温度、萃取时间和解析时间等关键因素。对于小于80目的烃源岩样品,推荐最优HS-SPME Arrow实验条件为:使用250μm PDMS箭形固相微萃取头, 120℃下萃取20 min, 260℃下解析8 min。对于稠油,当使用250μm PDMS萃取纤维头、萃取温度为120~150℃、萃取时间为15~20 min、解析时间为3~8 min时,稠油中的单金刚烷类和双金刚烷类化合物都能取得较理想的质谱响应。该方法实现了对烃源岩粉末和稠油中金刚烷类化合物的直接分析,灵敏度高,检出限低(0.004~0.977 ng/g),重现性好,测量峰面积和比值参数的相对标准偏差分别小于20%和5%,避免了复杂的前处理过程,是一种快捷可靠的分析方法。 展开更多
关键词 顶空箭形固相微萃取 气相色谱质谱 金刚烷类化合物 烃源岩 稠油
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液相色谱-串联质谱法测定土壤、沉积物和水中3种新型除草剂残留
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作者 何红梅 徐玲英 +5 位作者 张昌朋 方楠 蒋金花 王祥云 俞建忠 赵学平 《色谱》 CAS CSCD 北大核心 2024年第3期256-263,共8页
除草剂在杂草和有害植物防控上发挥着重要的作用,但其有效利用率低,大量除草剂进入环境中,对生态环境和人类健康构成了潜在威胁,因此建立环境样品中除草剂的残留分析方法尤为重要。该文采用电喷雾正离子源模式,建立了液相色谱-串联质谱... 除草剂在杂草和有害植物防控上发挥着重要的作用,但其有效利用率低,大量除草剂进入环境中,对生态环境和人类健康构成了潜在威胁,因此建立环境样品中除草剂的残留分析方法尤为重要。该文采用电喷雾正离子源模式,建立了液相色谱-串联质谱法(LC-MS/MS)测定土壤、沉积物和水中异噁唑草酮、吡唑草胺和苯嘧磺草胺残留量的方法。土壤和沉积物样品经乙腈振荡提取、盐析后经C18固相萃取小柱净化,水样过滤后经C_(18)固相萃取小柱净化;再用LC-MS/MS测定样品中异噁唑草酮、吡唑草胺和苯嘧磺草胺的残留量。实验优化了仪器检测和前处理条件,考察了方法的线性关系、基质效应、检出限和定量限,并选取4种土壤、2种沉积物和水样进行了方法验证。在0.0005~0.02 mg/L范围内,异噁唑草酮、吡唑草胺、苯嘧磺草胺的线性关系均良好,r≥0.9961。3种除草剂在土壤、沉积物和水中的基质效应为-10.1%~16.5%。异噁唑草酮、吡唑草胺和苯嘧磺草胺的检出限分别为0.05、0.02、0.01μg/kg,定量限分别为0.2、0.05、0.05μg/kg。异噁唑草酮、吡唑草胺和苯嘧磺草胺在土壤、沉积物和水样中3个水平(0.005、0.1、2.0 mg/kg)下的加标回收率分别为77.2%~101.9%、77.9%~105.1%、80.8%~107.1%;相对标准偏差(RSD)分别为1.4%~12.8%、1.2%~7.7%、1.5%~11.5%。结果表明:本方法操作简单,方法稳定,定量准确,实用性强,可用于土壤、沉积物和水中异噁唑草酮、吡唑草胺和苯嘧磺草胺残留量的检测。 展开更多
关键词 固相萃取 液相色谱-串联质谱 除草剂 土壤 沉积物
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基于壳聚糖改性的磁性氧化石墨烯的半自动化管尖固相微萃取技术在环境水中痕量铅快速测定中的应用
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作者 王露 张敏会 +3 位作者 王芹 宋鑫 冯晓青 杨鹏飞 《理化检验(化学分册)》 CAS CSCD 北大核心 2024年第10期965-972,共8页
以戊二醛为交联剂,采用壳聚糖(CS)和四氧化三铁(Fe_(3)O_(4))修饰氧化石墨烯(GO),制备了Fe_(3)O_(4)-GO/CS复合物(吸附剂)。将20 mg Fe_(3)O_(4)-GO/CS填装于200μL微型枪头中,两端填上少量玻璃棉,枪头旁边放置磁铁。将12 mL塑料注射器... 以戊二醛为交联剂,采用壳聚糖(CS)和四氧化三铁(Fe_(3)O_(4))修饰氧化石墨烯(GO),制备了Fe_(3)O_(4)-GO/CS复合物(吸附剂)。将20 mg Fe_(3)O_(4)-GO/CS填装于200μL微型枪头中,两端填上少量玻璃棉,枪头旁边放置磁铁。将12 mL塑料注射器和枪头连接,用塑料注射器吸取1 mL水冲洗Fe_(3)O_(4)-GO/CS表面可能吸附的杂质。环境水样经0.22μm滤膜过滤后,将滤液酸度调至pH6.0,用塑料注射器吸取10 mL,固定在注射泵上,将水样以0.8 mL·min^(-1)流量通过枪头;再吸取1 mL 0.010 mol·L^(-1)盐酸溶液(洗脱剂),以0.5 mL·min^(-1)流量洗脱吸附在Fe_(3)O_(4)-GO/CS上的铅。收集洗脱液,用电感耦合等离子体质谱法测定。结果显示:Fe_(3)O_(4)-GO/CS对铅的平衡吸附容量为126 mg·g^(-1),可重复使用50次,吸附过程符合朗缪尔(Langmuir)等温吸附模型;铅的质量浓度在0.01~10.00μg·L^(-1)内和响应值呈线性关系,检出限为0.005μg·L^(-1)。对实际水样进行3个浓度水平的加标回收试验,回收率为84.7%~105%,测定值的相对标准偏差(n=5)为0.90%~3.9%。 展开更多
关键词 石墨烯 壳聚糖 四氧化三铁 管尖固相微萃取 电感耦合等离子体质谱法
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