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Preparation and Characterization of Quercetin-Loaded Solid Dispersion by Solvent Evaporation and Freeze-Drying Method 溶剂蒸发-冷冻干燥法制备槲皮素负载固体分散体及表征
IF 0.5 Q4 SPECTROSCOPY Pub Date : 2016-09-30 DOI: 10.5478/MSL.2016.7.3.79
S. H. Park, I. Song, Min‐Koo Choi
We prepared solid dispersion formulations of quercetin to enhance its solubility and dissolution rate. Various quercetinloaded solid dispersion were tested with quercetin, poloxamer 407, and carrier such as hydroxypropyl methyl cellulose (HPMC), polyethylene glycol 8000 (PEG 8000), and polyvinylpyrrolidone K40 (PVP K40) using solvent evaporation and freeze drying methods in terms of both the aqueous solubility and the dissolution rates of quercetin. The solubility of quercetin as its solid dispersion formulations was markedly improved compared with that of quercetin powder. Especially, highest solubility of quercetin was observed when HPMC was used as a carrier. The cumulative dissolution of quercetin within 360 min from solid dispersion composed of quercetin, poloxamer 407, and HPMC was 8.8-fold higher than the dissolution of pure quercetin. The results of powder Xray diffraction (XRD) and scanning electron microscope (SEM) indicated that quercetin transformed from a crystalline to an amorphous form through the solid dispersion formulation process. These results suggest that the solid dispersion formulation of quercetin with poloxamer 407 and HPMC could be a promising option for enhancing the solubility and dissolution rate of quercetin.
为提高槲皮素的溶解度和溶出率,制备了槲皮素固体分散制剂。以槲皮素、poloxam407和羟丙基甲基纤维素(HPMC)、聚乙二醇8000 (PEG 8000)、聚乙烯吡咯烷酮K40 (PVP K40)为载体,采用溶剂蒸发和冷冻干燥的方法,对槲皮素的水溶性和溶出率进行了研究。槲皮素固体分散体的溶解度较槲皮素粉末有明显提高。特别是以HPMC为载体时,槲皮素的溶解度最高。槲皮素、poloxam407和HPMC组成的固体分散体在360 min内的累积溶出度是纯槲皮素的8.8倍。粉末x射线衍射(XRD)和扫描电镜(SEM)分析结果表明,槲皮素在固体分散配方过程中由结晶形态转变为无定形形态。上述结果表明,槲皮素与poloxam407和HPMC的固体分散是提高槲皮素溶解度和溶出率的一种有希望的选择。
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引用次数: 5
Identification of ML106 Phase 1 Metabolites in Human Liver Microsomes Using High-Resolution Quadrupole-Orbitrap Mass Spectrometry 用高分辨率四极轨道阱质谱法鉴定人肝微粒体中ML106 1期代谢物
IF 0.5 Q4 SPECTROSCOPY Pub Date : 2016-09-30 DOI: 10.5478/MSL.2016.7.3.69
J. Jo, W. Nam, Sunjoo Kim, Doohyun Lee, K. Min, Taeho Lee, Sangkyu Lee
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引用次数: 0
LC-MS/MS Method for Simultaneous Analysis of Growth Hormone-Releasing Peptides and Secretagogues in Human Urine LC-MS/MS同时分析人尿中生长激素释放肽和分泌物的方法
IF 0.5 Q4 SPECTROSCOPY Pub Date : 2016-09-30 DOI: 10.5478/MSL.2016.7.3.55
H. Min, Boyoung Han, Changmin Sung, K. Lee, H. Kim, Ki Hun Kim, J. Son, Jaeick Lee
Growth hormone (GH)-releasing peptides (GHRPs) and GH secretagogues (GHSs) are listed in the World Anti-Doping Agency (WADA) Prohibited List. In the present study, we developed and validated a method for the simultaneous analysis of seven GHRPs (alexamorelin, GHRP-1, -2, -4, -5, -6, and hexarelin) and three GHSs (anamorelin, ibutamoren, and ipamorelin) in human urine. Method validation was performed at minimum required performance levels specified by WADA technical documents (2 ng/mL) for all substances, and the method was validated with regard to selectivity (no interference), linearity (R2 > 0.9986), matrix effects (50.0%-141.2%), recovery (10.4%-100.8%), and intra- (2.8%-16.5%) and inter-day (7.0%-22.6%) precisions. The limits of detection for screening and confirmation were 0.05-0.5 ng/mL and 0.05-1 ng/mL, respectively.
生长激素(GH)释放肽(ghrp)和生长激素分泌物(GHSs)被列入世界反兴奋剂机构(WADA)禁用清单。在本研究中,我们开发并验证了一种同时分析人类尿液中7种ghrp(阿勒莫雷林、GHRP-1、-2、-4、-5、-6和hexarelin)和3种ghrp(阿纳莫雷林、伊布他莫林和伊帕莫雷林)的方法。在WADA技术文件规定的最低性能水平(2 ng/mL)下对所有物质进行方法验证,并对该方法进行了选择性(无干扰)、线性(R2 > 0.9986)、基质效应(50.0% ~ 141.2%)、回收率(10.4% ~ 100.8%)、内(2.8% ~ 16.5%)和日内(7.0% ~ 22.6%)精密度验证。筛选和确证的检出限分别为0.05 ~ 0.5 ng/mL和0.05 ~ 1 ng/mL。
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引用次数: 5
Differentiation of Glycan Diversity with Serial Affinity Column Set (SACS) 序列亲和柱集(SACS)对多糖多样性的鉴别
IF 0.5 Q4 SPECTROSCOPY Pub Date : 2016-09-30 DOI: 10.5478/MSL.2016.7.3.74
Jihoon Shin, W. Cho
Targeted glycoproteomics is an effective way to discover disease-associated glycoproteins in proteomics and serial affinity chromatography (SAC) using lectin and glycan-targeting antibodies shows glycan diversity on the captured glycoproteins. This study suggests a way to determine glycan heterogeneity and structural analysis on the post-translationally modified proteins through serial affinity column set (SACS) using four Lycopersicon esculentum lectin (LEL) columns. The great advantage of this method is that it differentiates between glycoproteins on the basis of their binding affinity. Through this study, some proteins were identified to have glycoforms with different affinity on a single glycoprotein. It will be particularly useful in determining biomarkers in which the disease-specific feature is a unique glycan, or a group of glycans.
靶向糖蛋白组学是蛋白质组学和序列亲和层析(SAC)中发现疾病相关糖蛋白的有效方法,利用凝集素和靶向糖聚糖的抗体可在捕获的糖蛋白上显示糖聚糖的多样性。本研究提出了一种利用4根番茄凝集素(LEL)序列亲和柱(SACS)测定翻译后修饰蛋白聚糖异质性和结构分析的方法。这种方法的最大优点是它根据糖蛋白的结合亲和力来区分糖蛋白。通过这项研究,一些蛋白质被鉴定出对单个糖蛋白具有不同亲和力的糖型。它将在确定疾病特异性特征是一个独特的聚糖或一组聚糖的生物标志物方面特别有用。
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引用次数: 1
Complete Simultaneous Analysis of Uranium Isotopes in NUSIMEP-7 Microparticles Using SEM-TIMS 用SEM-TIMS同时分析NUSIMEP-7微粒中的铀同位素
IF 0.5 Q4 SPECTROSCOPY Pub Date : 2016-09-30 DOI: 10.5478/MSL.2016.7.3.64
Jong-Ho Park, Kahee Jeong
: Scanning electron microscopy combined with thermal ionization mass spectrometry (SEM-TIMS) was used to determine the precise isotope ratios of ultra-trace levels of uranium contained in individual microparticles. An advanced multiple ion counter system consisting of three secondary ion multipliers and two compact discrete dynodes was used for complete simultaneous ion detection. For verification purposes, using TIMS with complete simultaneous measurement, isotopes were analyzed in 5 pg of uranium of a certified reference material. A microprobe in the SEM was used to transfer individual particles from a NUSIMEP-7 sample to TIMS filaments, which were then subjected to SEM-TIMS and complete simultaneous measurement. The excellent agreement in the resulting uranium isotope ratios with the certified NUSIMEP-7 values shows the validity of SEM-TIMS with complete simultaneous measurement for the analysis of uranium isotopes in individual particles. Further experimental study required for investigation of simultaneous measurement using the advanced multiple ion counter system is presented.
使用扫描电子显微镜结合热电离质谱(SEM-TIMS)来确定单个微粒中所含铀的超痕量水平的精确同位素比率。一个先进的多离子计数器系统由三个二次离子倍增器和两个紧凑的离散节点组成,用于完全同时检测离子。为了验证目的,使用TIMS进行完全同步测量,在经认证的参考物质的5 pg铀中分析了同位素。SEM中的微探针将NUSIMEP-7样品中的单个颗粒转移到TIMS细丝上,然后进行SEM-TIMS并完成同时测量。所得到的铀同位素比值与NUSIMEP-7的认证值非常吻合,表明SEM-TIMS可以完全同时测量单个颗粒中的铀同位素。提出了利用先进的多离子计数器系统进行同步测量的进一步实验研究。
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引用次数: 3
Recent Developments in Nuclear Forensic and Nuclear Safeguards Analysis Using Mass Spectrometry 质谱法在核法医和核保障分析中的最新进展
IF 0.5 Q4 SPECTROSCOPY Pub Date : 2016-06-30 DOI: 10.5478/MSL.2016.7.2.31
K. Song, Jong-Ho Park, Chi-Gyu Lee, Sun-ho Han
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引用次数: 3
UHPLC-ESI-qTOF-MS Analysis of Cyclopeptide Alkaloids in the Seeds of Ziziphus jujuba var. spinosa UHPLC-ESI-qTOF-MS分析酸枣种子中环肽生物碱
IF 0.5 Q4 SPECTROSCOPY Pub Date : 2016-06-30 DOI: 10.5478/MSL.2016.7.2.45
K. Kang, D. Jang, Jinwoong Kim, S. Sung
An UHPLC-ESI-qTOF-MS analytical method was developed for cyclopeptide alkaloids in the seeds of Ziziphus jujuba var. spinosa (Semen Ziziphi Spinosae), which is a commonly used herb in Chinese and Korean traditional medicines. Considering the basicity of cyclopeptide alkaloids, a specific separation method was developed for an UHPLC system. The compounds were detected by DAD and ESI-qTOF-MS, and their fragmentation patterns were also acquired by MS^{E} technologies. Peak-picking of major compounds was performed with nine previously isolated compounds and two reference standard compounds. Tandem MS fragmentation behaviors of type-Ia and -Ib cyclopeptide alkaloids were investigated with the acquired data to develop a strategy for dereplication of other cyclopeptide alkaloid compounds in Z. jujuba var. spinosa. Two more cyclopeptide alkaloids were tentatively identified with UHPLC-ESI-qTOF-MS using this method.
建立了一种hplc - esi - qtof - ms分析方法,分析了中药材中药材枣仁中环肽生物碱的含量。考虑到环肽生物碱的碱性,建立了一种高效液相色谱分离环肽生物碱的方法。通过DAD和ESI-qTOF-MS对化合物进行了检测,并通过MS^{E}技术获得了化合物的断裂模式。对9个先前分离的化合物和2个标准化合物进行了主要化合物的选峰。利用获得的数据研究了- ia型和-Ib型环肽生物碱的串联质谱断裂行为,以建立其他环肽生物碱化合物在枣树中的分离策略。并用UHPLC-ESI-qTOF-MS对另外两种环肽生物碱进行了初步鉴定。
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引用次数: 7
Improvement of Measurement Precisions for Uranium Isotopes at Ultra Trace Levels by Modification of the Sample Introduction System in MC-ICP-MS MC-ICP-MS样品导入系统改进对超痕量铀同位素测量精度的影响
IF 0.5 Q4 SPECTROSCOPY Pub Date : 2016-06-30 DOI: 10.5478/MSL.2016.7.2.50
Ranhee Park, S. Lim, Sun-ho Han, Min Young Lee, Jinkyu Park, Chi-Gyu Lee, K. Song
: Multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) is currently used in our laboratory for isotopic and quantitative analyses of nuclear materials at ultra-trace levels in environmental swipe samples, which is a very useful for monitoring undeclared nuclear activities. In this study, to improve measurement precisions of uranium isotopes at ultra-trace levels, we adopted a desolvating nebulizer system (Aridus-II, CETAC., USA), which can improve signal sensitivity and reduce formation of uranium hydride. A peristaltic pump was combined with Aridus-II in the sample introduction system of MC-ICP-MS to reduce long-term signal fluctuations by maintaining a constant flow rate of the sample solution. The signal sensitivity in the presence of Aridus-II was improved more than 10-fold and the formation ratio of UH/U decreased by 16- to 17-fold compared to a normal spray chamber. Long-term signal fluctuations were significantly reduced by using the peristaltic pump. Detailed optimizations and evaluations with uranium standards are also discussed in this paper.
多收集器电感耦合等离子体质谱(MC-ICP-MS)目前在我们的实验室中用于环境滑动样品中超痕量水平核材料的同位素和定量分析,这对于监测未申报的核活动非常有用。为了提高超痕量铀同位素的测量精度,本研究采用了一种脱溶雾化系统(Aridus-II, CETAC)。(美国),可以提高信号灵敏度,减少氢化铀的形成。在MC-ICP-MS的进样系统中,将蠕动泵与Aridus-II相结合,通过保持样品溶液的恒定流速来减少长期的信号波动。与普通喷雾室相比,Aridus-II存在时的信号灵敏度提高了10倍以上,UH/U的形成比降低了16 ~ 17倍。使用蠕动泵可显著降低长期信号波动。本文还详细讨论了用铀标准进行优化和评价的方法。
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引用次数: 3
Uranium Particle Identification with SEM-EDX for Isotopic Analysis by Secondary Ion Mass Spectrometry 二次离子质谱法鉴定铀粒子的SEM-EDX
IF 0.5 Q4 SPECTROSCOPY Pub Date : 2016-06-30 DOI: 10.5478/MSL.2016.7.2.41
F. Esaka, M. Magara
: Secondary ion mass spectrometry (SIMS) is a promising tool to measure isotope ratios of individual uranium particles in environmental samples for nuclear safeguards. However, the analysis requires prior identification of a small number of uranium particles that coexist with a large number of other particles without uranium. In the present study, this identification was performed by scanning electron microscopy - energy dispersive X-ray analysis with automated particle search mode. The analytical results for an environmental sample taken at a nuclear facility indicated that the observation of backscattered electron images with × 1000 magnification was appropriate to efficiently identify uranium particles. Lower magnification (less than × 500) made it difficult to detect smaller particles of approximately 1 µ m diameter. After identification, each particle was manipulated and transferred for subsequent isotope ratio analysis by SIMS. Consequently, the isotope ratios of individual uranium particles were successfully determined without any molecular ion interference. It was demonstrated that the proposed technique provides a powerful tool to measure individual particles not only for nuclear safeguards but also for environmental sciences.
次级离子质谱法(SIMS)是一种很有前途的工具,用于测量核保障环境样品中单个铀颗粒的同位素比率。但是,分析需要事先鉴定与大量其他无铀粒子共存的少量铀粒子。在本研究中,通过扫描电子显微镜-自动粒子搜索模式的能量色散x射线分析来进行这种鉴定。对某核设施环境样品的分析结果表明,观察× 1000倍放大的背散射电子图像可以有效地识别铀颗粒。较低的放大倍率(小于× 500)使得检测直径约为1 μ m的较小颗粒变得困难。鉴定后,每个粒子被处理并转移到随后的SIMS同位素比率分析。因此,在没有任何分子离子干扰的情况下,成功地确定了单个铀粒子的同位素比率。结果表明,所提出的技术不仅为核安全保障,而且为环境科学提供了测量单个粒子的有力工具。
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引用次数: 4
Dual Nano-Electrospray and Mixing in the Taylor Cone 双纳米电喷雾与泰勒锥混合
IF 0.5 Q4 SPECTROSCOPY Pub Date : 2016-03-31 DOI: 10.5478/MSL.2016.7.1.21
A. Radionova, D. Greenwood, G. Willmott, P. Derrick
Abstract : Dual-channel nano-electrospray has recently become an ionization technique of great promise especially in biologi-cal mass spectrometry. This unique approach takes advantage of the mixing processes that occurs during electrospray. Under-standing in more detail the fundamental principles influencing spray formation further study of the origins of the mixingprocesses: (1) in a Taylor cone region, (2) in charged droplets or (3) in both environments. The dual-channel emitters were mad efrom borosilicate theta-shape glass tubes (O.D. 1.2 mm) and had a tip diameters of less than 4µm. Electrical contact wasachived by deposition of a thin film of an appropriate metal onto the surface of the emitter. The experimental investigation ofthe Taylor cone formation in a dual-channel electrospray emitter has been carried out by injection of polystyrene beads(diameter 3µm) at very low concentrations into one of the channels of the non-tapered theta-glass tubes. High-speed cameraexperiments were set up to visualize the mixing processes in Taylor cone regions for dual-channel emitters. Mass spectra fromdual nano-electrospray are presented.Keywords : nano-electrospray, theta-shaped dual channel emitters, Taylor cone, mass spectrometry
摘要:近年来,双通道纳米电喷雾技术已成为一种极具发展前景的电离技术,特别是在生物质谱分析领域。这种独特的方法利用了电喷雾过程中发生的混合过程。更详细地了解影响喷雾形成的基本原理,进一步研究混合过程的起源:(1)在泰勒锥区域,(2)在带电液滴中,或(3)在两种环境中。双通道发射器由硼硅theta形玻璃管(外径1.2 mm)制成,尖端直径小于4µm。电接触是通过在发射极表面沉积一层适当的金属薄膜来实现的。采用极低浓度的聚苯乙烯微球(直径3µm)注入非锥形玻化管的一个通道中,对双通道电喷雾发射极中泰勒锥的形成进行了实验研究。建立了高速摄像实验,以可视化双通道发射器泰勒锥区域的混合过程。给出了双纳米电喷雾的质谱。关键词:纳米电喷雾,theta型双通道发射器,泰勒锥,质谱分析
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引用次数: 4
期刊
Mass Spectrometry Letters
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