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Analysis of Pesticide Raid^(█) in Feed of Wistar Rat by High-Pressure Liquid Chromatography (HPLC)
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作者 Albert C. Achudume 《American Journal of Analytical Chemistry》 2011年第8期32-36,共5页
The distribution of pesticide by-product in tissues of wistar rats were analyzed using high pressure liquid chromatography. The limit of detection of the HPLC was 0.1 μg. Results show bioaccumulation factor of pestic... The distribution of pesticide by-product in tissues of wistar rats were analyzed using high pressure liquid chromatography. The limit of detection of the HPLC was 0.1 μg. Results show bioaccumulation factor of pesticide “Raid?” in lipid, up to three times that of the feed at the first concentration and gradually decreased as the concentration increased in the muscle > (0.7), brain > (0.5) and liver > (0.3) as indicated in the text. At higher concentration of 961 μg/g, bioaccumulation factor decreased in the lipid to 1.2 and 0.6 in the muscle, 0.03 in the brain and 0.08 in the liver respectively. High Pressure Liquid Chromatography (HPLC) analysis of raid extract suggests the presence of micprothrin and palethrin. The implications are numerous, but simply put that accidental ingestion of chlorinated hydrocarbon as in “Raid?” may involve convulsions, collapse and coma after only brief excitation and ataxia at the onset. 展开更多
关键词 high pressure liquid chromatography PESTICIDE Raid^(█) Chlorinated Hydrocarbon BIOACCUMULATION
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Comparison of protocatechuic aldchyde in Radix Salvia miitiorrhiza and corresponding pharmacological sera from normal and fibrotic rats by high performance liquid chromatography 被引量:7
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作者 Tao Lv Xi-Xian Yao 《World Journal of Gastroenterology》 SCIE CAS CSCD 2006年第14期2195-2200,共6页
AIM: To observe the effect of protocatechuic aldchyde on the proliferation of hepatic stellate cells (HSCs). METHODS: Liver fibrosis was induced in rats by carbon tetrachloride (CCh). Then normal and fibrotic dr... AIM: To observe the effect of protocatechuic aldchyde on the proliferation of hepatic stellate cells (HSCs). METHODS: Liver fibrosis was induced in rats by carbon tetrachloride (CCh). Then normal and fibrotic drug sera were extracted from rats. The effects of protocatechuic aldchyde, raw Radix Salvia miltiorrhiza and drug sera of Salvia miltiorrhiza on HSC growth were determined by CCKoS. The protocatechuic aldchyde was separated by high performance liquid chromatography (HPLC) in a AIItima C18 column (250 mm × 4.6 mm, 5 μm) with a mobile phase of acetonitrile-4% glacial acetic acid solution (gradient elution) at the wavelength of 281 nm. RESULTS: Protocatechuic aldchyde, raw Radix Salvia miltiorrhiza and drug sera of Salvia miltiorrhiza were found to have inhibitory effects on proliferation of rat HSCs. Raw Radix Salvia miltiorrhiza had a stronger inhibitory effect than the drug sera. The fibrotic drug sera showed a higher suppressive effect than the normal drug sera (P 〈 0.05). Protocatechuic aldchyde was found in crude materials of both Radix Salvia miltiorrhiza and its corresponding drug sera. The average recovery (n = 6) was 110.5% for raw Salvia miltiorrhiza Bge, 102% for normal drug sera and 105.2% for fibrotic drug sera. The relative standard devitation (RSD) was 0.37%, 1.96% and 1.51%, respectively (n=6). The contents of protocatechuic aldchyde were 0.22%, 0.15% and 0.19%, respectively (n = 6) (P〈 0.05). The RSD was 0.33%, 0.75% and 1.24% (n=6) for raw material of Radix Salvia miltiorrhiza, normal drug sera and fibrotic drug sera, respectively. The samples were stable for 6 d. CONCLUSION: Protocatechuic aldchyde can inhibit the growth of HSCs. HPLC is suitable for the determination of virtual bioactive components of Chinese herbal medicines in vitro. 展开更多
关键词 Radix Salvia miltiorrhiza Protocatechuic aldchyde Seropharmacological method high performance liquid chromatography
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Development of a Fast and Facile Analytical Approach to Quantify Radiometabolites in Human Plasma Samples Using Ultra High Performance Liquid Chromatography
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作者 cile Malherbe +4 位作者 Rudy Bidault Claude Netter Denis Guilloteau Johnny Vercouillie Nicolas Arlicot 《American Journal of Analytical Chemistry》 2019年第5期185-201,共17页
Introduction: Conventional metabolite analyses often require manual sample preparation, generating variability of measurements. This study describes a new method to quantify radiometabolites in blood, combining ultra ... Introduction: Conventional metabolite analyses often require manual sample preparation, generating variability of measurements. This study describes a new method to quantify radiometabolites in blood, combining ultra high performance liquid chromatography (UHPLC) and turbulent flow chromatography, an alternative fully automated process allowing analyte’s extraction. Methods: A new radiotracer for dopamine transporter imaging, namely LBT-999, was used to demonstrate the method’s robustness. Matrix effect, Turboflow column loading, linearity, specificity and precision were evaluated with in vitro samples of LBT-999 in human plasma. Radiodetector sensitivity and preliminary evaluation were respectively determined by analysis of calibrated samples of [18F]LBT-999 and blood samples from 4 healthy subjects injected with [18F]LBT-999, withdrawn at 5, 15, 30 and 45 min pi. Results: With three sequential loadings (3 × 100 μL) of the Turboflow column, mean coefficients of variation were 1%, below 2%, 2% and 30.9% for matrix effect, specificity, repeatability and intermediate precision, respectively. Correlation coefficients for linearity were superior to 0.97. Limits of detection and quantification of the radiodetector were fixed at 3 and 9 c/s. Retention times for [18F]LBT-999 and the two radiometabolites detected by radio-UHPLC were 6.5, 4.8 and 9.6 min. Forty-five min after the injection, parent fraction was still predominant with 57.8% ± 25% of the total radioactivity. Conclusions: An innovative approach, allying UHPLC and Turboflow column, was developed and its sensitivity, linearity, specificity and repeatability validated. Preliminary results of the clinical trial are in accordance with literature data, demonstrating its efficiency in radiometabolites quantification. 展开更多
关键词 Radiometabolite ULTRA high Performance liquid chromatography Turboflow method Validation [18F]LBT-999
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Optimization of multicomponent solvent selection in high-performance liquid chromatography using a statistical method 被引量:1
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作者 WANG,Qin-Sun GAO,Ru-Yu WANG,Heng-Yan YAN,Bing-Wen National Laboratory of Elemento-Organic Chemistry,Nankai University,Tianjin 300071 《Chinese Journal of Chemistry》 SCIE CAS CSCD 1991年第3期222-230,共0页
A computer-assisted method is presented for optimization of multicomponent solvent mobile phase selection for separation of O-ethyl-N-isopropyl phosphoro(thioureido)thioates in reversed-phase HPLC and four geometric i... A computer-assisted method is presented for optimization of multicomponent solvent mobile phase selection for separation of O-ethyl-N-isopropyl phosphoro(thioureido)thioates in reversed-phase HPLC and four geometric isomers of pesticides Decis in normal-phase HPLC.The method is based on Snyder's solvent selection triangle concept using a statistical method.The optimization of the separation over the experimental region is based on a special polynomial esti- mation from seven experimental runs,and resolution(R_s)is used as the selection criterion.Excellent agreement was obtained between predicted data and experimental results. 展开更多
关键词 Optimization of multicomponent solvent selection in high-performance liquid chromatography using a statistical method high
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Advancements in the preparation of high-performance liquid chromatographic organic polymer monoliths for the separation of small-molecule drugs 被引量:5
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作者 Xiali Ding Jing Yang Yuming Dong 《Journal of Pharmaceutical Analysis》 SCIE CAS CSCD 2018年第2期75-85,共11页
The various advantages of organic polymer monoliths, including relatively simple preparation processes,abundant monomer availability, and a wide application range of pH, have attracted the attention of chromatographer... The various advantages of organic polymer monoliths, including relatively simple preparation processes,abundant monomer availability, and a wide application range of pH, have attracted the attention of chromatographers. Organic polymer monoliths prepared by traditional methods only have macropores and mesopores, and micropores of less than 50 nm are not commonly available. These typical monoliths are suitable for the separation of biological macromolecules such as proteins and nucleic acids, but their ability to separate small molecular compounds is poor. In recent years, researchers have successfully modified polymer monoliths to achieve uniform compact pore structures. In particular, microporous materials with pores of 50 nm or less that can provide a large enough surface area are the key to the separation of small molecules. In this review, preparation methods of polymer monoliths for high-performance liquid chromatography, including ultra-high cross-linking technology, post-surface modification, and the addition of nanomaterials, are discussed. Modified monolithic columns have been used successfully to separate small molecules with obvious improvements in column efficiency. 展开更多
关键词 high-PERFORMANCE liquid chromatography Polymer MONOLITH Preparation methods Small molecules
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Plasma amino acid profiling of cancer patients with abnormal Savda based on high-performance liquid chromatography 被引量:1
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作者 Batur Mamtimin Kedena +5 位作者 Bin Kong Ayshamgul Hasim Aynur Matsidik Mawlanjan Hizbulla Nazuk Kurbantay Halmurat Upur 《Journal of Traditional Chinese Medicine》 SCIE CAS CSCD 2014年第5期560-565,共6页
OBJECTIVE: To investigate metabolic signatures in plasma of cancer patients with abnormal Savda using plasma-free amino acid profiles, and to evaluate the diagnostic potential of these profiles for the detection and e... OBJECTIVE: To investigate metabolic signatures in plasma of cancer patients with abnormal Savda using plasma-free amino acid profiles, and to evaluate the diagnostic potential of these profiles for the detection and explanation of the mechanisms of different symptoms in traditional Uyghur medicine.METHODS: Plasma samples from cancer patients with abnormal Savda(n=85) or non-abnormal Savda(n=105) and a healthy control group(n=65)were analyzed using high-performance liquid chromatography(HPLC). Orthogonal projection to latent structures with discriminant analysis was used for the classification and prediction of abnormal Savda, and spectral profiles were subjected to Student's t-tests to assess statistical significance.RESULTS: Compared with the healthy group, the levels of aspartic acid, glutamate, glycine, histidine,arginine, threonine, alanine, proline, methionine,isoleucine, leucine and phenylalanine decreased significantly in plasma of cancer patients with abnormal Savda(all P<0.05). Serine, cystine, tyrosine,valine and lysine levels showed no significant differences(all P>0.05). Compared with non-abnormal Savda syndrome patients, abnormal Savda syndrome patients showed high concentrations of glutamate, serine, valine, isoleucine, leucine and phenylalanine(all P<0.05). The remaining plasma amino acids showed no significant differences(all P>0.05).CONCLUSION: Plasma-free amino acid profiling has the potential to assist in understanding and determining abnormal Savda. A HPLC-based metabonomic platform could be a powerful tool for the classification of symptoms in traditional medicine. 展开更多
关键词 Amino acids Medicine Uyghur tradi-tional chromatography high pressure liquid Ab-normal Savda
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Comparison between different methods of estimation of vitamin D 被引量:1
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作者 Mrinal Pal Subinay Datta +7 位作者 Amit Kumar Pradhan Lekha Biswas Joydeep Ghosh Partha Mondal Rajarshi Rahut Arghya Ray Chaudhuri Sourav Sau Soumi Das 《Advances in Biological Chemistry》 2013年第5期501-504,共4页
Background: Vitamin D is not only important for bone health but can also affect the development of several non-bone diseases. These findings have increased the need for determining vitamin D status in a convenient and... Background: Vitamin D is not only important for bone health but can also affect the development of several non-bone diseases. These findings have increased the need for determining vitamin D status in a convenient and cost-effective way. In order to determine the better method for detecting vitamin D status, we have estimated blood vitamin D in three methods such as high-pressure liquid chromatography, chemiluminescent immunoassays and enzyme immunoassays. Method: Two hundred and sixteen subjects irrespective of age and sex were studied for blood vitamin D in all the three methods over a period of 2 years. Result: The statistical analysis showed that values of vitamin D obtained by chemiluminescent immunoassays (r = 0.978, 展开更多
关键词 VITAMIN D high-pressure liquid chromatography Chemiluminescent Immunoassays ENZYME Immunoassays
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Relationship between cardiotonic activity of Fuzi(Radix Aconiti Lateralis Preparata)and its fingerprint determined by liquid chromatography-mass spectrometry
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作者 TONG Hengli ZHU Jing +2 位作者 ZHONG Lingyun XU Ting GONG Feipeng 《Journal of Traditional Chinese Medicine》 SCIE CSCD 2021年第1期140-149,共10页
OBJECTIVE:To investigate the relationship between the cardiotonic activity of Fuzi(Radix Aconiti Lateralis Preparata,RALP)and its fingerprint determined by liquid chromatography-mass spectrometry(LC-MS).METHODS:First,... OBJECTIVE:To investigate the relationship between the cardiotonic activity of Fuzi(Radix Aconiti Lateralis Preparata,RALP)and its fingerprint determined by liquid chromatography-mass spectrometry(LC-MS).METHODS:First,the fingerprints of six processed products of RALP were established by high performance liquid chromatography quadrupole time-of-flight mass spectrometry(HPLC-Q-TOF-MS)followed by analysis of the principal component of the relative peak area of its common peaks.Next,the scores of the first five principal components were used as input for an artificial neural network(ANN).Additionally,the therapeutic effect of RALP was assessed by measuring the hemodynamic indexes of heart failure model rats.Subsequently,fluorescence semi-quantitative polymerase chain reaction and an enzyme-linked immunosorbent assay kit were used to determine the effects of RALP-processed products on the serum levels of noradrenaline(NA),angiotensin-Ⅰ(Ang-Ⅰ),and the expression ofβ-norepinephrine receptor m RNA(β-NRm)in the rat cardiac tissues.P<0.05 was used as the output of the ANN.Finally,a network was constructed to display the relationship between the LC-MS fingerprints and the cardiotonic activity of the RALP-processed products.RESULTS:Several types of RALPs can improve diastolic function,systolic function and heart rate.On the basis of the findings from the principal component analysis(PCA)of 16 common peaks of fingerprints of six RALP-processed products,it was revealed that the first five principal components may include 100%of the information of the original data.As observed from the multilayer perceptron neural network analysis,principal component 4 presented with the strongest effects on serum levels of NA and Ang-Ⅰin rats,while principal component1 exerted the greatest effect onβ-NRm expression in cardiac tissue.CONCLUSION:The key findings obtained from this study indicated that the network constructed by the PCA-ANN may predict pharmacodynamic effects of the main ingredients of Traditional Chinese Medicine(TCM).This method may serve as a new approach to identify the relationship between LC-MS fingerprints and the pharmacodynamic effects of TCM ingredients. 展开更多
关键词 chromatography high pressure liquid Mass spectrometry Principal component analysis Radix Aconiti Lateralis Preparata GINGER Artificial neural network
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Establishment of a Method for Determination of Anemoside B4 Content in Pulsatilla Water Extract 被引量:2
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作者 王建舫 《Agricultural Science & Technology》 CAS 2015年第8期1600-1602,共3页
[Objective] This study aimed to establish a new method for determination of anemoside B4 content in pulsatilla water extract. [Method] Using acetonitrile-water (28:72) as the mobile phase, the high performance liqu... [Objective] This study aimed to establish a new method for determination of anemoside B4 content in pulsatilla water extract. [Method] Using acetonitrile-water (28:72) as the mobile phase, the high performance liquid chromatography, equipped with UV detector, was used to determine the anemoside B4 content in pulsatilla water extract. [Result] In the concentration range of 300-800 μg/ml, anemoside B4 content showed a good linear relationship with peak area. The average recovery of anemoside B4 was 98.12% (n=-6; RSD=-1.37%). [Conclusion] The established method meets the requirements by methodology, and it can be used to determine the anemoside B4 content in pulsatilla water extract. 展开更多
关键词 Pulsatilla Anemoside B4 high performance liquid chromatography method establishment
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Determination of S/R ratio of mephenytoin in human urine by chiral HPLC and ultraviolet detection and its comparison with gas chromatography 被引量:4
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作者 黄松林 谢红光 +3 位作者 王伟 许振华 蒋长虹 周宏灏 《中国药理学报》 CSCD 1998年第6期548-550,共3页
目的:建立人尿中R,S美芬妥英的液相色谱手性分离与检测方法,用于CYP2C19酶活性的快速测定.方法:受试者口服消旋美芬妥英后的0-8h尿液标本用二氯甲烷提取后用手性色谱柱进行分离,流动相为乙腈和水(14∶86,体... 目的:建立人尿中R,S美芬妥英的液相色谱手性分离与检测方法,用于CYP2C19酶活性的快速测定.方法:受试者口服消旋美芬妥英后的0-8h尿液标本用二氯甲烷提取后用手性色谱柱进行分离,流动相为乙腈和水(14∶86,体积比),其中含有0.1%的冰醋酸和0.2%的三乙胺,流速为0.9mL·min-1,紫外检测波长为207nm.结果:在选定的色谱条件下R,S美芬妥英能很好地分离,尿中其他物质无干扰.用外标法定量,线性范围在50-5000μg·L-1,最小检出浓度为12.5μg·L-1,保留时间在9min内.液相色谱分析结果和气相色谱分析具有良好的一致性.结论:该法样本制备简便、分析时间短、线性范围宽、干扰少、灵敏和准确。 展开更多
关键词 美芬妥英 高压液相色谱 气相色谱 尿检测
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干燥方式对山楂总黄酮含量及抗氧化性质的影响
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作者 娄世豪 孙小晶 +2 位作者 李丹丹 赵晨晨 修建华 《食品工业科技》 CAS 北大核心 2025年第1期121-129,共9页
本研究采用热风干燥、真空冷冻干燥及热风联合液氮干燥对山楂进行处理,利用亚硝酸钠-硝酸铝-氢氧化钠显色法、高效液相色谱法和自由基清除能力实验研究不同干燥方式对山楂粉样品的总黄酮得率、总黄酮组分和含量及抗氧化活性的影响。结... 本研究采用热风干燥、真空冷冻干燥及热风联合液氮干燥对山楂进行处理,利用亚硝酸钠-硝酸铝-氢氧化钠显色法、高效液相色谱法和自由基清除能力实验研究不同干燥方式对山楂粉样品的总黄酮得率、总黄酮组分和含量及抗氧化活性的影响。结果表明,热风干燥、真空冷冻干燥和热风联合液氮干燥的山楂粉样品色差值分别为20.60、17.70、20.05;山楂总黄酮得率分别为64.59、71.48、60.77 mg/g;对DPPH自由基清除率分别是19.56%、30.14%、18.50%;对ABTS+自由基清除率分别是51.81%、75.08%、48.68%;以及对羟自由基清除率分别是48.98%、55.77%、36.04%;真空冷冻干燥处理的山楂粉样品中总黄酮得率较高,具有较强的抗氧化活性,且与其它样品具有显著性差异(P<0.05);同时高效液相色谱对山楂总黄酮进行定性和定量分析结果表明,三种干燥方式得到的黄酮类物质均包含芦丁、金丝桃苷、杨梅素、槲皮素、芹菜素、异鼠李素,但其含量不同,真空冷冻干燥样品中总黄酮总含量达到了308.65 mg/g,与其他样品具有显著性差异(P<0.05)。除此以外,三种抗氧化方式和六种组分含量之间也存在线性关系。综上考虑,真空冷冻干燥处理山楂,是提取山楂总黄酮的推荐方法,可以有效减少对山楂的总黄酮含量及抗氧化活性的影响。 展开更多
关键词 山楂 总黄酮 干燥方式 抗氧化活性 扫描电镜 高效液相色谱
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A Stability Indicating Reverse Phase-HPLC Method Development and Validation for the Estimation of Rucaparib in Bulk and Pharmaceutical Dosage Form 被引量:1
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作者 D. Suchitra Satyanarayana Battu 《American Journal of Analytical Chemistry》 2021年第4期96-107,共12页
The research was carried out for establishing a new reverse phase-HPLC stability indicating method for the quantification of Rucaparib. The experiment was determined on Waters HPLC instrument using 996 photo-diode arr... The research was carried out for establishing a new reverse phase-HPLC stability indicating method for the quantification of Rucaparib. The experiment was determined on Waters HPLC instrument using 996 photo-diode array detector. The separation was done by using symmetry C-18 ODS (25 cm × 0.46 cm internal diameter) 5 μm analytical column containing mobile phase of Phosphate buffer (0.02 M) and methanol [65:35% v/v] adjusted pH to 4.8 by adding dilute ortho phosphoric acid. The method was run at 1 ml·min<sup>-1</sup> at 286 nm detection. The drug was eluted at 5.484 min. After developing the method, it was assured for the intended use by validation which was done according to ICH Q2B guidelines. The analytical parameters checked were linearity, accuracy, repeatability, intermediate precision, limit of detection, limit of quantitation, ruggedness and robustness. It was observed that the response of the detector was linear in the range of 6 - 14 μg/ml with correlation coefficient of 0.999. The results of all the parameters were found to be within the acceptance criteria. The stability indicating assay method was established by using the samples generated by forced degradation process. The forced degradation was carried out by subjecting the drug to acid, alkali, thermal, oxidative and photolytic degradation and the results showed that the degradation products were successfully separated from the drug. Hence, this can be applied perfectly later for the analysis of quality of the rucaparib drug. 展开更多
关键词 Rucaparib Reverse-Phase high Performance liquid chromatography method Development VALIDATION
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A Stability Indicating Reverse Phase-HPLC Method Development and Validation for the Estimation of Bimatoprost 0.3% &Timolol 0.5% Pharmaceutical Ophthalmic Dosage Form
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作者 Md. S. Amin Muhammad T. Islam 《American Journal of Analytical Chemistry》 CAS 2022年第12期506-530,共25页
The research was carried out to establish a new reverse phase-HPLC stability indicating method for quantifying Bimatoprost & Timolol in ophthalmic solution. The experiment of Bimatoprost & Timolol in ophthalmi... The research was carried out to establish a new reverse phase-HPLC stability indicating method for quantifying Bimatoprost & Timolol in ophthalmic solution. The experiment of Bimatoprost & Timolol in ophthalmic solution method development was determined on Waters HPLC instrument using a UV Detector. The separation was done by using L11, Zorbex SB phenyl (4.6 mm × 250 mm internal diameter) 5 μm analytical column, containing mobile phase of Phosphate buffer (0.02 M), methanol, and acetonitrile [50:30:20 % v/v]. The method was run at 1 ml·min<sup>-1</sup> at 210 nm for Bimatoprost and 295 nm for Timolol for detection. The drug was eluted at 10.81 min for Bimatoprost and 3.77 min for Timolol. After developing the method, it was assured for the intended use by validation, which was done according to ICH Q2B guidelines. The analytical parameters checked were Specificity/Selectivity, linearity, Range, accuracy, ruggedness, and robustness. It was observed that the response of the detector was linear in the range of 6 - 18 μg/ml with a correlation coefficient of 0.999. The results of all the parameters were found to be within the acceptance criteria. The stability-indicating assay method was established by using the samples generated by the forced degradation process. The forced degradation was carried out by subjecting the drug to acid, alkali, thermal, oxidative, and photolytic degradation, and the results showed that the degradation products were successfully separated from the drug. Hence, this can be applied perfectly later for the quantitative analysis of Bimatoprost 0.3% + Timolol 0.5% Ophthalmic Solution drugs for pharmaceutical use. Currently, there is no official method for Bimatoprost & Timolol combination products in USP or BP. Available research work related to single Bimatoprost or Timolol products was not suitable for testing Bimatoprost and Timolol combination drugs. Additionally, there is no stability-indicating method to test Bimatoprost & Timolol combination products which insist us to do research and develop a new reverse phase-HPLC indicating method which will be faster and more accurate. 展开更多
关键词 BIMATOPROST TIMOLOL Reverse-Phase high Performance liquid chromatography method Development Validation Stability Indicating
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UPLC-MS/MS法检测3种食品中松仁过敏原 被引量:1
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作者 宁亚维 周泓鑫 +4 位作者 杨正 马俊美 刘茁 张岩 李强 《食品科学》 EI CAS CSCD 北大核心 2024年第1期247-253,共7页
基于食品基质中松仁过敏原Pin k 2建立了一种超高效液相色谱-串联质谱法。将松仁经过研磨、脱脂、浸提、酶解后经Easy-nLC 1000-QExactive高分辨质谱仪进行分离分析,结合Uniprot蛋白数据库以及ProteinPilotTM软件对质谱图进行数据处理,... 基于食品基质中松仁过敏原Pin k 2建立了一种超高效液相色谱-串联质谱法。将松仁经过研磨、脱脂、浸提、酶解后经Easy-nLC 1000-QExactive高分辨质谱仪进行分离分析,结合Uniprot蛋白数据库以及ProteinPilotTM软件对质谱图进行数据处理,经BLAST验证特异性,最终筛选3条松仁特异性肽段。方法学验证结果表明,方法在0.001~50mg/mL范围内线性关系良好,定量限为1mg/kg;在饼干、巧克力和饮料3种空白基质中的平均回收率为88.50%~107.57%,相对标准偏差不高于6.08%,基质效应为89.77%~96.13%。该方法具有灵敏度高、特异性好的优势,可应用于饼干、巧克力、饮料等食品样品中松仁过敏原的检测,为我国食品标签真实性检验及食品中隐性过敏原的检测提供技术支持。 展开更多
关键词 松仁 过敏原 超高效液相色谱-串联质谱法 检测
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不同产地杜仲叶活性成分的定量分析 被引量:1
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作者 龚频 柯瀛瀛 +4 位作者 翟鹏涛 翟文俊 李白存 郑本忠 崔梦娇 《陕西科技大学学报》 北大核心 2024年第4期70-77,共8页
通过杜仲叶中主要活性成分绿原酸的提取率,优化杜仲叶活性成分的提取工艺,比较不同产地杜仲叶组成及含量的差异.以绿原酸为目标产物,通过单因素实验和Box-Behnken模型,并采用高效液相色谱法测定秦仲叶和华仲叶中芦丁、松脂醇二葡萄糖苷... 通过杜仲叶中主要活性成分绿原酸的提取率,优化杜仲叶活性成分的提取工艺,比较不同产地杜仲叶组成及含量的差异.以绿原酸为目标产物,通过单因素实验和Box-Behnken模型,并采用高效液相色谱法测定秦仲叶和华仲叶中芦丁、松脂醇二葡萄糖苷、金丝桃苷、绿原酸及没食子酸五种活性成分含量.单因素条件对两者叶的提取效果影响均为:提取温度>提取时间>乙醇体积分数>料液比.在最佳提取条件下,秦仲叶绿原酸提取率为62.94%,华仲叶绿原酸提取率为47.84%.两者叶中绿原酸含量最高,秦仲叶中芦丁、松脂醇二葡萄糖苷含量比华仲叶高出1.97倍和6.59倍,但华仲叶中金丝桃苷和绿原酸含量比秦仲叶高出1.41倍和1.16倍.本研究旨在为不同地域杜仲树种的选育以及临床上应用标准提供理论依据,帮助更加全面地评价不同产地杜仲药材质量. 展开更多
关键词 绿原酸 响应面法 高效液相色谱 不同产地 定量
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盾尾刷更换时液氮冻结温度场及冻结参数影响的数值模拟分析 被引量:1
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作者 杨平 毛一祥 姚梦威 《隧道建设(中英文)》 CSCD 北大核心 2024年第1期69-77,共9页
为合理确定高水压下液氮冻结止水更换盾尾刷的冻结设计参数及掌握温度场变化规律,结合某过江通道长距离盾构掘进过程中盾尾刷更换时的液氮冻结止水工程,利用ADINA大型有限元分析软件建立液氮冻结止水及盾尾刷更换数值模型,模拟温度-时... 为合理确定高水压下液氮冻结止水更换盾尾刷的冻结设计参数及掌握温度场变化规律,结合某过江通道长距离盾构掘进过程中盾尾刷更换时的液氮冻结止水工程,利用ADINA大型有限元分析软件建立液氮冻结止水及盾尾刷更换数值模型,模拟温度-时间变化曲线与现场实测数据对比,验证模型的合理性,并对土层、去路液氮温度、冻结管长度、冻结管间距、冻结方式进行敏感性因素分析。结果表明:1)冻结效果随土层的不同而发生改变,在卵石层、砾砂层、粉细砂层3种土层中,粉细砂层的冻结效果最差,卵石层最好;2)在有限的冻结时间内,去路液氮温度的不同,只影响土体从开始冻结至越过0℃完成相变这期间的降温速度,不影响完成冻结以后的土体降温速率;3)冻结管长度对土层冻结的影响较小,可以采用较短的冻结管,以降低施工成本和液氮消耗量,但不能过短,应保证其纵向有足够的支撑范围,经计算分析,当冻结管长度为1.52 m时,能在轴面处满足2.0 m的冻结壁厚度要求;4)冻结管间距对冻结效果影响大,冻结管越密,冻结速度越快,效果越好;5)在相同条件下,双环预埋冻结管液氮冻结效果优于管片上直接打孔液氮冻结。 展开更多
关键词 高水压砂性地层 盾尾刷更换 液氮冻结法 数值分析 温度场
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高效液相色谱-串联四极杆质谱法测定人参组培不定根中11种皂苷成分
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作者 董喆 王玉梅 +3 位作者 孙姗姗 曹进 李梦怡 高飞 《化学分析计量》 CAS 2024年第10期55-62,共8页
建立高效液相色谱-串联四极杆质谱(HPLC-MS/MS)法定量分析人参组培不定根中11种皂苷成分。样品经粉碎研磨,以70%甲醇水溶液为溶剂进行超声提取,离心过滤后测定。采用C_(18)色谱柱(100 mm×2.1 mm,1.8μm),用水和乙腈进行梯度洗脱,... 建立高效液相色谱-串联四极杆质谱(HPLC-MS/MS)法定量分析人参组培不定根中11种皂苷成分。样品经粉碎研磨,以70%甲醇水溶液为溶剂进行超声提取,离心过滤后测定。采用C_(18)色谱柱(100 mm×2.1 mm,1.8μm),用水和乙腈进行梯度洗脱,流量为0.3 mL/min,柱温为35℃。质谱采用电喷雾电离源,负离子扫描,多反应监测模式进行检测。11种皂苷的质量浓度在0.1~10μg/mL(Rb1为0.2~10μg/mL)范围内和响应强度线性相关,相关系数均大于0.995,各皂苷的定量限为0.001~0.010 g/kg,加标回收率为90.43%~97.82%,相对标准偏差为1.93%~6.33%(n=6)。该方法操作简单,分析时间短,灵敏度高,准确可靠,适用于人参组培不定根中多种皂苷类成分的同时测定。 展开更多
关键词 高效液相色谱-串联四极杆质谱法 人参组培不定根 皂苷
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高效液相色谱-串联质谱法检测牛组织和奶中咪多卡残留的研究
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作者 白玉惠 孙红洋 +3 位作者 张骊 朱馨乐 沈昕 黄耀凌 《中国兽药杂志》 2024年第4期69-75,共7页
建立了一种检测牛组织和牛奶中咪多卡残留检测的高效液相色谱-串联质谱法。牛组织(肌肉、肝脏、肾脏、脂肪)和奶在NaAc缓冲体系中酶解,经HCl溶液提取,WCX固相萃取柱净化,以0.3%甲酸水溶液(含20 mM甲酸铵)和0.3%甲酸乙腈为流动相进行梯... 建立了一种检测牛组织和牛奶中咪多卡残留检测的高效液相色谱-串联质谱法。牛组织(肌肉、肝脏、肾脏、脂肪)和奶在NaAc缓冲体系中酶解,经HCl溶液提取,WCX固相萃取柱净化,以0.3%甲酸水溶液(含20 mM甲酸铵)和0.3%甲酸乙腈为流动相进行梯度洗脱,在HILIC色谱柱上分离,在电喷雾正离子(ESI^(+))模式下,用多反应监测(MRM)模式检测,同位素内标法定量。结果表明:咪多卡在2.5~1000 ng/mL的浓度范围内呈现良好线性关系,相关系数(R^(2))大于0.99;咪多卡在牛组织和奶中的检测限均为10μg/kg,定量限均为20μg/kg;咪多卡在牛组织和奶中20~4000μg/kg添加浓度水平上的回收率在70.9%~109%范围内;批内RSD在0.55%~9.59%之间,批间RSD在2.21%~12.1%之间。该方法具有灵敏度高、定量准确,重复性好等特点,可以满足牛组织和奶中咪多卡残留检测的要求。 展开更多
关键词 牛组织 牛奶 咪多卡 残留 高效液相色谱-串联质谱法
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高效液相色谱内标法测定海水叶绿素a浓度
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作者 李芝凤 杨安安 +1 位作者 韩冰 郭凯 《海洋技术学报》 2024年第4期56-62,共7页
叶绿素a浓度是海水水质监测和海洋赤潮预警的重要指标,高效液相色谱法作为叶绿素a浓度最准确的测量方法之一被广泛应用。本文选用β-阿朴-8’-胡萝卜素醛(β-Apocarotena-8’-carotenal,Apocarotenal)为内标物,建立了一种基于液相色谱... 叶绿素a浓度是海水水质监测和海洋赤潮预警的重要指标,高效液相色谱法作为叶绿素a浓度最准确的测量方法之一被广泛应用。本文选用β-阿朴-8’-胡萝卜素醛(β-Apocarotena-8’-carotenal,Apocarotenal)为内标物,建立了一种基于液相色谱内标法的海水叶绿素a浓度分析方法,在实验检测范围内,方法相关性良好,相关系数为0.9998,检出限为0.05μg/L,回收率为97.0%~100%,相对标准偏差为0.38%~0.55%,精密度良好。同时,利用实验室培养的小球藻藻液和现场海水样品对内标法和外标法进行了显著性差异评估。结果表明:两种方法不存在显著性差异,12组现场海水样品内标法和外标法的测定结果相关性良好,相关系数为0.92,平均相对误差为6.21%。液相色谱内标法测定海水叶绿素a浓度分离效果好、准确度高,能对实验室叶绿素a浓度的测量进行较为准确的质量控制。 展开更多
关键词 高效液相色谱 内标法 叶绿素A 显著性差异评估
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配合饲料中64种药物超高效液相色谱-三重四极杆串联质谱检测方法的研究
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作者 陈海燕 陈娟 +4 位作者 李永琴 马春芳 张慧宁 杨俊华 杨奇 《畜牧与饲料科学》 2024年第3期11-19,共9页
[目的]建立同时检测配合饲料中64种药物的超高效液相色谱-三重四极杆串联质谱(ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry,UHPLC-MS/MS)法,提高非法添加物的检测效率。[方法]采用Waters... [目的]建立同时检测配合饲料中64种药物的超高效液相色谱-三重四极杆串联质谱(ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry,UHPLC-MS/MS)法,提高非法添加物的检测效率。[方法]采用Waters HSS T3型色谱柱(2.1 mm×100 mm,1.8μm)进行分离,流动相A为0.1%甲酸水溶液,流动相B为含0.1%甲酸的乙腈溶液,梯度洗脱,流速为0.40 mL/min,进样量为2μL;采用电喷雾离子源正离子扫描模式进行检测,多反应监测模式进行信号采集。比较4种样品提取溶剂以及2种固相萃取柱处理对目标药物的回收率,确定样品前处理的最佳方法。利用建立的UHPLC-MS/MS法对宁夏回族自治区不同来源的100批次配合饲料样品进行64种药物检测。[结果]配合饲料样品均质后,用含0.2%甲酸的乙腈水溶液(乙腈∶水=8∶2,V/V)提取,利用Oasis PRiME HLB型固相萃取柱对样品净化,多数目标药物的回收率在60%以上。64种药物在浓度为5.0~200.0μg/L的范围内线性关系良好,相关系数(R)均大于0.99;不同药物的定量限在5.0~10.0μg/kg;阳性添加5.0、20.0、50.0μg/kg 3个浓度的平均回收率在41.00%~120.49%,批内相对标准偏差(RSD)在0.54%~15.94%,批间RSD在1.25%~13.64%。在100个批次的配合饲料样品中均未检出目标药物。[结论]建立的UHPLC-MS/MS法线性关系良好、回收率高、精密度好,具有较高的重现性和较好的可操作性,可用于配合饲料中非法添加64种药物的筛查。 展开更多
关键词 配合饲料 超高效液相色谱-三重四极杆串联质谱法 非法添加 兽药
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