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固相萃取-气相色谱-质谱法同时测定水中9种药品及个人护理用品 被引量:25
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作者 贾妍艳 谭建华 +3 位作者 徐晨 汤嘉骏 王赢利 解启来 《色谱》 CAS CSCD 北大核心 2014年第3期263-267,共5页
采用固相萃取-气相色谱-质谱联用技术,建立了水体中9种药品及个人护理用品(水杨酸、萘普生、布洛芬、对乙酰氨基酚、降固醇酸、三氯生、双氯酚酸、酮洛芬和双酚 A)的定量分析方法。水样品经稀盐酸调节至 pH =3后,采用 Oasis HLB 固... 采用固相萃取-气相色谱-质谱联用技术,建立了水体中9种药品及个人护理用品(水杨酸、萘普生、布洛芬、对乙酰氨基酚、降固醇酸、三氯生、双氯酚酸、酮洛芬和双酚 A)的定量分析方法。水样品经稀盐酸调节至 pH =3后,采用 Oasis HLB 固相萃取小柱进行富集净化;选用三甲基氢氧化硫( TMSH)为衍生化试剂,在常温条件下对目标物进行快速甲基化;以气相色谱-质谱法选择离子监测模式(GC-MS-SIM)进行检测,由2,4,5-涕丙酸为内标进行定量分析。本实验分别对固相萃取和衍生化等前处理条件进行了系统的研究。在优化的实验条件下,方法的回收率为50.7~115.4%,相对标准偏差均不高于10%,检出限为0.03~0.30μg / L,定量限为0.15~1.50μg / L。利用该方法对东莞市某农田灌溉水进行了分析,4种目标物在样品中有检出,最大质量浓度范围为0.176~0.998μg / L。结果表明该方法操作简便,灵敏可靠。 展开更多
关键词 固相萃取 衍生化 气相色谱-质谱联用 药品及个人护理用品 水样 solid phase extraction(SPE) gas chromatography-mass spectrom-etry(GC-MS) pharmaceuticals and personal care products(PPCPs)
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固相萃取-超高效液相色谱-电喷雾串联质谱法同时测定地表水中16种全氟有机化合物 被引量:23
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作者 张明 唐访良 +3 位作者 俞雅雲 陈峰 徐建芬 叶永根 《色谱》 CAS CSCD 北大核心 2014年第5期472-476,共5页
建立了固相萃取-超高效液相色谱-电喷雾串联三重四极杆质谱联用技术分析水中16种全氟有机化合物的高通量检测方法。样品经 WAX 固相萃取柱富集和净化后,采用 Waters ACQUITY UPLCTM BEH C18色谱柱,含2 mmol/L乙酸铵的甲醇和含2 mmol/... 建立了固相萃取-超高效液相色谱-电喷雾串联三重四极杆质谱联用技术分析水中16种全氟有机化合物的高通量检测方法。样品经 WAX 固相萃取柱富集和净化后,采用 Waters ACQUITY UPLCTM BEH C18色谱柱,含2 mmol/L乙酸铵的甲醇和含2 mmol/L乙酸铵的水作为流动相进行梯度洗脱,质谱采用电喷雾负离子电离,多反应监测模式检测。16种全氟有机化合物在0.5~100μg/L或1.0~100μg/L 浓度范围内线性关系良好,相关系数为0.9987~0.9999,方法的检出限为0.06~0.46 ng/L;高、中、低3个添加水平的回收率为67.6%~103%,相对标准偏差为2.94%~12.0%。结果表明,该方法灵敏、准确且检测范围广,分析速度快,是一种适于实际水样中全氟有机化合物检测分析的方法。 展开更多
关键词 固相萃取 超高效液相色谱 电喷雾串联质谱 全氟有机化合物 地表水 solid phase extraction( SPE) ultra performance liquid chromatography( UPLC) ELECTROSPRAY IONIZATION tandem mass spectrometry( ESI-MS MS)
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福建姜黄挥发油化学成分的HS-SPME-GC-MS分析 被引量:18
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作者 强悦越 韦航 +4 位作者 方灵 吴妙鸿 谭索 曾绍校 傅建炜 《中国食品添加剂》 CAS 2020年第1期147-153,共7页
采用水蒸气蒸馏法提取福建姜黄挥发油,应用顶空固相微萃取进样结合气相色谱-串联质谱联用技术(HS-SPME-GC-MS)分析姜黄挥发油的化学成分。结果表明:姜黄挥发油含有量为7.2%(mL/g),从姜黄挥发油中共分出62个色谱峰,初步鉴定出了其中的51... 采用水蒸气蒸馏法提取福建姜黄挥发油,应用顶空固相微萃取进样结合气相色谱-串联质谱联用技术(HS-SPME-GC-MS)分析姜黄挥发油的化学成分。结果表明:姜黄挥发油含有量为7.2%(mL/g),从姜黄挥发油中共分出62个色谱峰,初步鉴定出了其中的51种化学成分,占总挥发油总量的98.41%。在鉴定的化合物中,主要为单萜类化合物和倍半萜类化合物,其中新发现一种主要成分为β-柏木烯,相对含量占比高达26.58%,这可作为福建姜黄挥发油的特征成分和主要品质指标。本研究结果将为福建姜黄植物药材的品质评价提供科学依据。 展开更多
关键词 姜黄挥发油 顶空固相微萃取技术(Head space solid phase micro-extraction HS-SPME) 气相色谱-质谱联用技术(Gas chromatography-mass spectrometry GC-MS) 化学成分
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Aroma changes of black tea prepared from methyl jasmonate treated tea plants 被引量:13
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作者 Jiang SHI Li WANG +3 位作者 Cheng-ying MA Hai-peng LV Zong-mao CHEN Zhi LIN 《Journal of Zhejiang University-Science B(Biomedicine & Biotechnology)》 SCIE CAS CSCD 2014年第4期313-321,共9页
Methyl jasmonate(MeJA) was widely applied in promoting food quality.Aroma is one of the key indicators in judging the quality of tea.This study examined the effect of exogenous MeJA treatment on tea aroma.The aroma ... Methyl jasmonate(MeJA) was widely applied in promoting food quality.Aroma is one of the key indicators in judging the quality of tea.This study examined the effect of exogenous MeJA treatment on tea aroma.The aroma components in black tea prepared from MeJA-treated fresh tea leaves were extracted using headspace solid-phase microextraction(HS-SPME) and were analyzed using gas chromatography-mass spectrometry(GC-MS) and GC-olfactometry(GC-O).Forty-five volatile compounds were identified.The results revealed that the MeJA-treated black tea had higher levels of terpene alcohols and hexenyl esters than the untreated tea.Moreover,several newly components,including copaene,cubenol,and indole,were induced by the MeJA treatment.The activities of polyphenol oxidase and β-glucosidase in fresh tea leaves changed after the MeJA treatment.Quantitative real-time polymerase chain reaction(qRT-PCR) analysis indicated that the gene expression levels of polyphenol oxidase and β-primeverosidase were upregulated by two and three folds,respectively,by the MeJA treatment(P0.01); however,the gene expression of β-glucosidase was downregulated to a half level.In general,the aroma quality of the MeJAtreated black tea was clearly improved. 展开更多
关键词 AROMA Black tea Methyl jasmonate(MeJA) Headspace solid-phase microextraction(HS-SPME) Gas chromatography-mass spectrometry(GC-MS) Gas chromatography-olfactometry(GC-O) Gene expression
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Comprehensive Mathematical Model for Coal Combustion in a Circulating Fluidized Bed Combustor 被引量:9
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作者 金晓钟 吕俊复 +3 位作者 杨海瑞 刘青 岳光溪 冯俊凯 《Tsinghua Science and Technology》 SCIE EI CAS 2001年第4期319-325,共7页
Char combustion is on a special reducing condition in the dense bed of a circulating fluidized bed combustor. Experimental findings were used to develop a comprehensive mathematical model to simulate the hydrodynami... Char combustion is on a special reducing condition in the dense bed of a circulating fluidized bed combustor. Experimental findings were used to develop a comprehensive mathematical model to simulate the hydrodynamic and combustion processes in a circulating fluidized bed combustor. In the model, gas solid interaction was used to account for the mass transfer between the bubble phase and the emulsion phase in the dense bed, which contributes to the reducing atmosphere in the dense bed. A core annular structure was assumed in the dilute area rather than a one dimensional model. The submodels were combined to build the comprehensive model to analyze the combustion in a circulating fluidized bed combustor and the effect of operating parameters on the coal combustion. The model predictions agree well with experimental results. 展开更多
关键词 reducing condition gas solid mass transfer volatiles release core annular
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固体质量流量测量技术进展 被引量:10
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作者 董群 王丽 +1 位作者 任东海 张国甲 《化工进展》 EI CAS CSCD 北大核心 2010年第S2期1-4,共4页
气固两相流中的固体质量流量的测量对节能有重要的意义,但固体质量流量的测量一直是一个亟需解决的难题。本文主要介绍了几种国内外研究中比较热的、最有发展前途的测量方法,并对其进行阐述,并且简单的介绍了固体流量测量的发展方向。
关键词 气固两相流 固体质量 测量 多相流
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Identification and Characterization of Sulfur Compounds in Straight-Run Diesel Using Comprehensive Two-Dimensional GC Coupled with TOF MS 被引量:10
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作者 Niu Luna Liu Zelong Tian Songbai 《China Petroleum Processing & Petrochemical Technology》 SCIE CAS 2014年第3期10-18,共9页
The solid-phase extraction using Pd-Al2O3 as the stationary phase was employed to pre-separate the sulfur compounds in straight-run diesel. The isolating effect was evaluated quantitatively by gas chromatography with ... The solid-phase extraction using Pd-Al2O3 as the stationary phase was employed to pre-separate the sulfur compounds in straight-run diesel. The isolating effect was evaluated quantitatively by gas chromatography with a sulfur chemiluminescence detector to harvest a satisfactory result. The identification of the structure of sulfur compounds by comprehensive two-dimensional gas chromatography coupled with the time-of-flight mass spectrometry indicated that cyclo-sulfides, benzothiophenes, dibenzothiophenes, dihydro-benzothiophenes and tetrahydro-dibenzothiophenes were included in straightrun diesel obtained from the Arab medium crude(AM). A total of 259 individual compounds were detected and their molecular structures were identified. The analytical method was approved as an effective way to characterize the composition of sulfur compounds, which reduced the interference of other compounds, facilitated the data presentation and provided more detailed information about molecular composition of sulfur compounds. 展开更多
关键词 sulfur compounds straight-run diesel solid-phase extraction (SPE) comprehensive two-dimensional gas chromatographycoupled with the time-of-flight mass spectrometry (GC×GC-TOF MS)
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气相色谱-负化学源质谱联用法测定水产品及食用油中氟乐灵的残留量 被引量:9
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作者 王莉 夏广辉 +5 位作者 沈伟健 吴斌 张睿 陆慧媛 沈崇钰 赵增运 《色谱》 CAS CSCD 北大核心 2014年第3期314-317,共4页
建立了一种可用于水产品及食用油中氟乐灵残留量分析的分散型固相萃取-气相色谱-负化学离子源质谱方法。水产品及食用油经乙腈提取,4℃冷藏后,采用分散型固相萃取法净化,由气相色谱-负化学离子源质谱选择离子监测技术进行测定与确证... 建立了一种可用于水产品及食用油中氟乐灵残留量分析的分散型固相萃取-气相色谱-负化学离子源质谱方法。水产品及食用油经乙腈提取,4℃冷藏后,采用分散型固相萃取法净化,由气相色谱-负化学离子源质谱选择离子监测技术进行测定与确证,同位素内标法定量。在1~40μg / L 范围内氟乐灵农药的线性关系良好;方法定量限(LOQ)为0.02μg / kg;对鳗鱼、烤鳗、梭子蟹、小龙虾、猪油和橄榄油等6种复杂基质进行1.0、2.0和3.0μg / kg 等3个水平的添加回收试验,平均回收率均处于80%~100%之间,RSD≤10.3%;无干扰现象出现。该方法可作为水产品及食用油中氟乐灵残留检测的确证方法。 展开更多
关键词 分散型固相萃取 气相色谱-负化学离子源质谱联用 选择离子监测 氟乐灵 水产品 食用油 disperse solid phase extraction( DSPE) gas chromatography-negative chemical ionization mass SPECTROMETRY ( GC-MS NCI ) selected ion monitoring ( SIM )
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Adult pancreatoblastoma: Current concepts in pathology 被引量:9
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作者 Ayo O Omiyale 《World Journal of Gastroenterology》 SCIE CAS 2021年第26期4172-4181,共10页
Adult pancreatoblastoma is an exceptionally rare malignant tumour of the pancreas that mimics other solid cellular neoplasms of the pancreas,which may pose diagnostic difficulties.Because of its rarity,little is known... Adult pancreatoblastoma is an exceptionally rare malignant tumour of the pancreas that mimics other solid cellular neoplasms of the pancreas,which may pose diagnostic difficulties.Because of its rarity,little is known about its clinical and pathologic features.This article reviews the clinical and pathologic features of pancreatoblastoma in adults including differential diagnosis,treatment,and follow-up.Although pancreatoblastoma commonly occurs in childhood,there have now been more than 70 adult pancreatoblastomas described in the literature.There is a slight male predominance.There are no symptoms unique to pancreatoblastomas and adult patients are frequently symptomatic.The most common presenting symptom is abdominal pain.Grossly,the tumours are often large and well-circumscribed.Microscopically,pancreatoblastomas are composed of neoplastic cells with predominantly acinar differentiation and characteristic squamoid nests.These tumours are positive for trypsin,chymotrypsin,lipase,and BCL10.Loss of heterozygosity on chromosome 11p is the most common molecular alteration in pancreatoblastomas.Adult pancreatoblastomas are aggressive tumours with frequent local invasion,recurrence,and distant metastasis.Treatment consists of surgical resection.Chemotherapy and radiotherapy may have a role in the treatment of recurrent,residual,unresectable,and metastatic disease.It is important to distinguish pancreatoblastomas from morphological mimics such as acinar cell carcinomas,solid pseudopapillary neoplasms,and pancreatic neuroendocrine neoplasms. 展开更多
关键词 PANCREAS Adult pancreatoblastoma Pancreatic cancer solid pancreatic mass Non-ductal pancreatic tumours
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Comparison of simultaneous distillation extraction and solid-phase micro-extraction for determination of volatile constituents in tobacco flavor 被引量:8
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作者 钟科军 魏万之 +1 位作者 郭方遒 黄兰芳 《Journal of Central South University of Technology》 EI 2005年第5期546-551,共6页
The volatile and semi-volatile components in tobacco flavor additives were extracted by both simultaneous distillation extraction and solid-phase micro-extraction. Extraction conditions for solid-phase micro-extractio... The volatile and semi-volatile components in tobacco flavor additives were extracted by both simultaneous distillation extraction and solid-phase micro-extraction. Extraction conditions for solid-phase micro-extraction were optimized with information theory. Then, detection were accomplished by gas chromatography-mass spectrometry. Characteristic of each method was compared. Qualitative analysis and quantitative analysis of 6# tobacco flavor sample were accomplished through both simultaneous distillation extraction and solid-phase micro-extraction. The experimental results show that solid-phase micro-extraction method is the first choice for qualitative analysis and simultaneous distillation extraction is another good selection for quantitative analysis. By means of simultaneous distillation extraction, 20 components are identified, accounting for 92.77% of the total peak areas. Through solid-phase micro-extraction, there are 17 components identified accounting for 91.49% of the total peak areas. The main aromatic components in 6# tobacco flavor sample are propanoic acid, 2-hydroxy-, ethyl ester, menthol and menthyl acetate. The presented method has been successfully used for quality control of tobacco flavor. 展开更多
关键词 simultaneous distillation extraction solid-phase micro-extraction gas chromatography-mass spectrometry tobacco flavor
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颗粒对液-固二相润滑摩擦和温度特性影响的试验研究 被引量:6
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作者 刘伟 刘小君 +1 位作者 王伟 刘焜 《合肥工业大学学报(自然科学版)》 CAS CSCD 北大核心 2009年第5期624-627,639,共5页
文章研究了润滑油中含有固体颗粒时对摩擦副摩擦和温度特性的影响,试验在HDM20端面摩擦磨损试验机上进行,试验采用3种微米级的固体颗粒添加剂,即Al2O3、MoS2和石墨粉,在线测量了温度的变化过程和摩擦系数;结果表明,较软的MoS2和石墨粉... 文章研究了润滑油中含有固体颗粒时对摩擦副摩擦和温度特性的影响,试验在HDM20端面摩擦磨损试验机上进行,试验采用3种微米级的固体颗粒添加剂,即Al2O3、MoS2和石墨粉,在线测量了温度的变化过程和摩擦系数;结果表明,较软的MoS2和石墨粉降低了温度,减小摩擦系数,较硬的Al2O3颗粒升高了温度,容易使摩擦副擦伤;颗粒加入量对温度和摩擦特性有明显影响,在该文研究工况下,1.5μm的石墨粉质量分数控制在5%以内对润滑有一定改善作用,在1%时效果最好。选用1.5μm、2.3μm、4.0μm、10μm、15μm、30μm粒径的石墨颗粒进行了试验研究,发现从1.5-4.0μm时,随着颗粒粒径的增大温度变高,摩擦系数变大,从4-30μm时,随着颗粒粒径的增大温度变低,摩擦系数变小。 展开更多
关键词 固体颗粒 质量分数 颗粒粒径 温度 润滑
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21 0 2型农用柴油机平衡性分析及平衡措施 被引量:6
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作者 毕玉华 申立中 何自力 《昆明理工大学学报(理工版)》 2002年第1期86-88,共3页
利用I -DEAS三维实体造型软件的参数化技术 ,建立了 2 1 0 2型农用柴油机曲轴飞轮总成的三维模型 .通过对两缸机的平衡性进行计算 ,分析了现有两缸机平衡性存在的问题 。
关键词 曲轴 平衡性 三维实体
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Isolated Cells of Porphyra yezoensis Cultured on Solid Medium 被引量:4
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作者 Shen Songdong(沈颂东) +1 位作者 Dai Jixun(戴继勋) 《Marine Science Bulletin》 CAS 2001年第1期45-50,共6页
Vegetative cells of Porphyra yezoensis are isolated with sea snail enzyme and cultured on the solidified agar medium. The results of experiments show that the isolated cells can survive,divide and regenerate well on t... Vegetative cells of Porphyra yezoensis are isolated with sea snail enzyme and cultured on the solidified agar medium. The results of experiments show that the isolated cells can survive,divide and regenerate well on the medium solidified with agar. The first division on the solid medium starts after 7 days' culture, 4 days later than the liquid culture. The survival rate of isolated cells is 71.3% on the solid medium, lower than the 86.2% of that in seawater.Thalli, thalloids,conchocelis, spermatangia and multicellular masses are developed on the solid/medium in the first month, slowly but normally. Spermatangia sacs disappear within 4 weeks. Without adding nutrient liquid onto the surface of solid medium or injecting seawater under the agar layer in order to keep moisture, the thalli and cell groups release monospores to form new thalli instead of enlarging their areas after 5 weeks' culturing. Some monospores regenerate new thalli. Other monospores lose their pigments and minimize their volume and divide quickly to form light pink calli. After 16 weeks, numerous calli can be seen on the solid medium and after 24 weeks' culturing, almost only calli and conchocelis can be seen. If the calli are immersed in seawater, the monospores are released and may develop into young thallus. 展开更多
关键词 solid culture PORPHYRA yezoensis thallus callus multicellular mass development
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Automatic analytical approach for the determination of 12 illicit drugs and nicotine metabolites in wastewater using on-line SPE-UHPLC-MS/MS 被引量:6
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作者 Jingyuan Wang Likai Qia +8 位作者 Chenzhi Hou Tingting Zhang Mengyi Chen Haitao Meng Mengxiang Su Hui Xu Zhendong Hua Youmei Wang Bin Di 《Journal of Pharmaceutical Analysis》 SCIE CAS CSCD 2021年第6期739-745,共7页
In this study,we developed a novel on-line solid phase extraction(SPE)-ultra-high-performance liquid chromatography tandem mass spectrometry(UHPLC-MS/MS)-based analytical method for simultaneously quantifying 12 illic... In this study,we developed a novel on-line solid phase extraction(SPE)-ultra-high-performance liquid chromatography tandem mass spectrometry(UHPLC-MS/MS)-based analytical method for simultaneously quantifying 12 illicit drugs and metabolites(methamphetamine,amphetamine,morphine,codeine,6-monoacetylmorphine,benzoylecgonine,3,4-methylenedioxymethamphetamine,3,4-methylenedioxyamphetamine,cocaine,ketamine,norketamine,and methcathinone)and cotinine(COT)in wastewater samples.The analysis was performed by loading 2 m L of the sample onto an Oasis hydrophilic-lipophilic balance cartridge and using a cleanup step(5%methanol)to eliminate interference with a total run time of 13 min.The isotope-labeled internal standard method was used to quantify the target substances and correct for unavoidable losses and matrix effects during the on-line SPE process.Typical analytical characteristics used for method validation were sensitivity,linearity,precision,repeatability,recovery,and matrix effects.The limit of detection(LOD)and limit of quantification(LOQ)of each target were set at 0.20 ng/L and 0.50 ng/L,respectively.The linearity was between 0.5 ng/L and250 ng/L,except for that of COT.The intra-and inter-day precisions were<10.45%and 25.64%,respectively,and the relative recovery ranged from 83.74%to 162.26%.The method was used to analyze various wastewater samples from 33 cities in China,and the results were compared with the experimental results of identical samples analyzed using off-line SPE.The difference rate was between 19.91%and-20.44%,and the error range could be considered acceptable.These findings showed that on-line SPE is a suitable alternative to off-line SPE for the analysis of illicit drugs in samples. 展开更多
关键词 Illicit drugs and metabolites Wastewater analysis On-line solid phase extraction Ultra-high-performance liquid CHROMATOGRAPHY mass spectrometry
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Numerical Simulation of the Mass Movement Process of the 2018 Sedongpu Glacial Debris Flow by Using the Fluid-Solid Coupling Method 被引量:1
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作者 Xing-Yu Long Yu-Xiang Hu +1 位作者 Bin-Rui Gan Jia-Wen Zhou 《Journal of Earth Science》 SCIE CAS CSCD 2024年第2期583-596,共14页
In the context of global warming and intensified human activities,glacier instability in plateau regions has increased,and glacier debris flows have become active,which poses a significant threat to the lives and prop... In the context of global warming and intensified human activities,glacier instability in plateau regions has increased,and glacier debris flows have become active,which poses a significant threat to the lives and property of people and socioeconomic development.The mass movement process of glacier debris flows is extremely complex,so this paper uses the 2018 Sedongpu glacier debris flow event on the Qinghai-Tibet Plateau as an example and applies a numerical simulation method to invert the whole process of mass movement.In view of the interaction between phases in the process of motion,we use the fluid-solid coupling method to describe the mass movement.The granular-flow model and drift-flux model are employed in FLOW3D software to study the mass movement process of glacier debris flows and explore their dynamic characteristics.The results indicate that the glacier debris flow lasted for 700 s,and the movement process was roughly divided into four stages,including initiation,scraping,surging and deposition;the depositional characteristics calculated by the fluid-solid coupling model are consistent with the actual survey results and have good reliability;strong erosion occurs during the mass movement,the clear volume amplification effect,and the first wave climbs 17.8 m across the slope.The fluid-solid coupling method can better simulate glacier debris flows in plateau regions,which is helpful for the study of the mechanism and dynamic characteristics of such disasters. 展开更多
关键词 glacial debris flow Qinghai-Tibet Plateau fluid-solid coupling FLOW3D mass movement depositional characteristics DISASTERS engineering geology
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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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Identification of Active Components in Humic Acids Affecting Tomato Germination
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作者 Wei Shiping Shi Peihua +4 位作者 Wang Quanzhi Wang Yuanhua Zhao Jiayin Yin Kaijun Wu Meng 《Journal of Northeast Agricultural University(English Edition)》 CAS 2024年第4期1-15,共15页
Humic acids can promote the germination of many vegetable seeds,but the key active components remain unclear.This study utilized nutrient content,cross polarization magic angle spin ^(13)C solid magnetic resonance(CPM... Humic acids can promote the germination of many vegetable seeds,but the key active components remain unclear.This study utilized nutrient content,cross polarization magic angle spin ^(13)C solid magnetic resonance(CPMAS-^(13)C-NMR)and ultra-high performance liquid chromatography-mass spectrometry(UHPLC-MS)to characterize the chemical components of humic acids.Tomato seed germination index(GI)was determined with the goal of screening the key active components of humic acids.Humic acids had a significantly higher nutrient content,except for the total nitrogen(TN)and the total phosphorus(TP)contents.Humic acids had a higher content of O-CH_(3)/NCH,aromatic C-O and carbonyl C compared to weathered coal,with significantly lower anomeric C,aromatic C and O-alkyl C/alkyl C.There were 611 different compounds identified among the test materials using UHPLC-MS.Humic acids also had a significantly higher GI(158.0%and 153.1%)than weathered coal(85.5%).The organic matter(OM),TP and available potassium(AK)contents in humic acids were significantly positively correlated with GI,and available phosphorus(AP)was significantly negatively correlated.Among the carbon components,O-CH3/NCH,aromatic C-O and O-alkyl C/alkyl C were significantly positively correlated with GI,while anomeric C was significantly negatively correlated.Furthermore,among the top 10 positive and five negative correlation compounds,lipids and lipid-like molecules[armexifolin,boviquinone 4,3-methyladipic acid,lxocarpalactone A,monic acid,DG(20:1(11Z)/18:4(6Z,9Z,12Z,15Z)/0:0),and brassinolide]and organic acids and derivatives(N-acetylglutamic acid,8-hydroxy-5,6-octadienoic acid,acetyl-L-tyrosine,and hydroxyprolyl-methionine)in humic acids might be crucial active components for improving tomato seed germination.The results provided direct evidence for the identification of bioactive molecules of humic acids,and a scientific basis for the precise utilization of bioactive molecular components of humic acids in sustainable agricultural development. 展开更多
关键词 humic acid cross polarization magic angle spin 13C solid magnetic resonance(CPMAS-13C-NMR) ultra-high performance liquid chromatography-mass spectrometry(UHPLC-MS) germination index(GI) active component
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Detection of Endocrine Disruptors in Water around Landfills
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作者 Dandan LIU Qing LI +4 位作者 Yaohong LIU Sha FENG Tao MO Zheng LIU Xiaonan ZOU 《Agricultural Biotechnology》 2024年第1期66-70,73,共6页
[Objectives]This study was conducted to explore the occurrence levels of endocrine disruptors(EDCs)in rural areas around a county landfill in Tongren City.[Methods]The water around the landfill was sampled and analyze... [Objectives]This study was conducted to explore the occurrence levels of endocrine disruptors(EDCs)in rural areas around a county landfill in Tongren City.[Methods]The water around the landfill was sampled and analyzed.A solid-phase extraction and high performance liquid chromatography-tandem mass spectrometry(SPE-UPLC-MS/MS)method was established for the determination of 27 EDCs.After the HLB solid-phase extraction column was activated,a water sample,which was adjusted with phosphoric acid to a pH of 2(±0.5)and added with 500 mg of disodium EDTA,was loaded,and 5 ml of water and 20%methanol water was added for washing.Next,10 ml of elution solution was added for elution,and the collected eluate was evaporated under reduced pressure at 40℃to near dryness,and 1 ml of reconstitution solution was added to a constant volume.An ACQUITY UPLC BEH C18(100×2.1 mm,2.6μm)chromatographic column was adopted for LC separation by gradient elution with pure water solution-acetonitrile as the mobile phase.For MS detection,the MRM mode was adopted for collection,and the positive and negative ion modes were switched for simultaneous determination,and the internal standard method was used for quantification.[Results]The correlation coefficient R2 was greater than 0.99 in the linear range of each target substance.The limits of quantitation in the method were between 0.05 and 2.00 ng/L,and the recoveries ranged from 75.3%to 105.7%.[Conclusions]The method has high sensitivity,good accuracy and strong practical value. 展开更多
关键词 LANDFILL Endocrine disruptor solid phase extraction High performance liquid chromatography-tandem mass spectrometry
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Determination of Ten Kinds of Alpha-2 Agonists Residues in Animal Derived Food by UHPLC-Triple Quadrupole/Composite Linear Ion Trap Mass Spectrometry
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作者 Fang LI Xuemei LI +3 位作者 Xiangang LI Sining LIU Sha LIU Ying WANG 《Plant Diseases and Pests》 2024年第1期28-32,共5页
[Objectives]The paper was to establish an ultra high performance liquid chromatography-quadrupole/linear ion trap complex mass spectrometry for the determination of 10 kinds ofα2-receptor agonists in animal derived f... [Objectives]The paper was to establish an ultra high performance liquid chromatography-quadrupole/linear ion trap complex mass spectrometry for the determination of 10 kinds ofα2-receptor agonists in animal derived food.[Methods]The samples were extracted with sodium carbonate buffer solution and ethyl acetate,and analyzed by mass spectrometry after solid phase extraction and high performance liquid chromatography separation.[Results]Ten kinds ofα2-receptor agonists showed a good linear relationship in the range of 1-100μg/mL,with the average recovery of over 69%and the relative standard deviation less than 8.32%.The detection limit of 10 kinds of α_(2)-receptor agonists was up to 1μg/kg.[Conclusions]The method has good selectivity and strong anti-interference ability,and can meet the requirements of 10 kinds ofα2-receptor agonists residues in animal derived food. 展开更多
关键词 Animal derived food α_(2)-receptor agonist solid-phase extraction Ultra-high performance liquid phase-triple quadrupole/linear ion trap composite mass spectrometry
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An efficient resin for solid-phase extraction and determination by UPLCMS/MS of 44 pharmaceutical personal care products in environmental waters 被引量:4
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作者 Feng Zhu Zhijian Yao +5 位作者 Wenliang Ji Deye Liu Hao Zhang Aimin Li Zongli Huo Qing Zhou 《Frontiers of Environmental Science & Engineering》 SCIE EI CAS CSCD 2020年第3期177-187,共11页
In this study,a hydrophilic resin named GCHM was fabricated based on poly(N-vinyl pyrrolidone-codivinylbenzene),characterized,and applied as a solid-phase extraction(SPE)material.Up to 44 pharmaceuticals and personal ... In this study,a hydrophilic resin named GCHM was fabricated based on poly(N-vinyl pyrrolidone-codivinylbenzene),characterized,and applied as a solid-phase extraction(SPE)material.Up to 44 pharmaceuticals and personal care products(PPCPs)belonging to 10 classes were recovered in environmental water samples.Different variables affecting extraction,such as adsorbent amount,sample pH,and loading speed,were optimized.Under optimal conditions,the average absolute recovgy of 44 PPCPs was 75.6%using GCHM,indicating a better performance than the commercial Oasis^HLB.SPE with home-made hydrophilic polymeric sorbent followed by ultra-performance liquid chromatography and tandem mass spectrometry was validated,and the method achieved good linearity(r2>0.991,for all analytes).In addition,the method detection limits of target compounds ranged from 0.03 to 0.6 ng/L.The developed method was applied to determine PPCPs in 10 environmental water samples taken from the Yangtze River,Huaihe River,and Taihu Lake,1 groundwater sample from Changzhou in Jiangsu Province,1 wastewater sample from Xiamen and 2 seawater samples from the Jiulong River in Fujian Province,China.In these samples,22 compounds were determined at levels ranging from 0.5 to 1590 ng/L. 展开更多
关键词 Hydrophilic resin solid phase extraction Pharmaceuticals and personal care product Ultra-performance liquid chromatography and tandem mass spectrometry Environmental water
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