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Journal of Separation Science

Yi Tao, Yingshan Du, Dandan Su, Weidong Li, Baochang Cai
A rapid and sensitive ultra high performance liquid chromatography with tandem mass spectrometry approach was established for the simultaneous determination of 4-caffeoylquinic acid, loganic acid, chlorogenic acid, loganin, 3,5-dicaffeoylquinic acid, dipsacoside B, asperosaponin VI and sweroside in raw and wine-processed Dipsacus asper. Chloramphenicol and glycyrrhetinic acid were employed as internal standards. The proposed approach was fully validated in terms of linearity, sensitivity, precision, repeatability as well as recovery...
February 20, 2017: Journal of Separation Science
Sainan Li, Jianxu Zhang, Senlin Li, Chunming Liu, Shu Liu, Zhiqiang Liu
Stroke is one of the most common diseases worldwide. Lactate dehydrogenase inhibitors are widely used in the treatment of ischemic stroke, with natural products considered a promising source of lactate dehydrogenase inhibitors. In this study, ultrafiltration liquid chromatography coupled with mass spectrometry was used for the screening and identification of lactate dehydrogenase inhibitors from Poria cocos. Five lactate dehydrogenase inhibitors were selected: dehydropachymic acid, pachymic acid, dehydrotrametenolic acid, trametenolic acid, and eburicoic acid...
February 20, 2017: Journal of Separation Science
Shengqiang Tong, Xiaoping Wang, Mangmang Shen, Liqiong Lv, Mengxia Lu, Zhisi Bu, Jizhong Yan
3-Phenyllactic acid is an antimicrobial compound with broad-spectrum activity against various bacteria and fungus. The observed difference in pharmacological activity between optical isomeric 3-phenyllactic acid necessitates a method for enantioseparation. Chiral ligand exchange countercurrent chromatography was investigated for the enantioseparation of 3-phenyllactic acid with a synthesized chiral ligand. A two-phase solvent system was composed of n-butanol/hexane/water (0.4:0.6:1, v/v/v) to which N-n-dodecyl-l-hydroxyproline was added to the organic phase as chiral ligand and cupric acetate was added in the aqueous phase as a transitional metal ion...
February 20, 2017: Journal of Separation Science
Nela Šestáková, Regula Theurillat, Parham Sendi, Wolfgang Thormann
Cefepime monitoring in deproteinized human serum and plasma by micellar electrokinetic capillary chromatography and liquid chromatography coupled to mass spectrometry in presence of other drugs is reported. For micellar electrokinetic capillary chromatography, sample preparation comprised dodecylsulfate protein precipitation at pH 4.5 using an increased buffer concentration compared to that of a previous assay and removal of hydrophobic compounds with dichloromethane. This provided robust conditions for cefepime analysis in the presence of sulfamethoxazole and thus enabled its determination in samples of patients that receive co-trimoxazole...
February 20, 2017: Journal of Separation Science
Xian-Long Cheng, Qian-Qian Zhang, Ming-Hua Li, Hua Yan, Kun-Zi Yu, Jian-Li Zhou, Li Shao-Ping, Feng Wei, Shuang-Cheng Ma
An ultra high performance liquid chromatography with quadrupole time-of-flight mass spectrometry method coupled with principal component analysis was developed and applied to the identification of Cornu Antelopis, Cornu Bubali, Cornu Naemorhedi, and Cornu Bovis. The data obtained from the trypsin-digested samples were subjected to principal component analysis to classify these four cornua. Additionally, marker peptides of the cornua were determined by orthogonal partial least-squares discriminant analysis, and fragmentation tandem mass spectra of these marker peptides were evaluated...
February 20, 2017: Journal of Separation Science
Rafael R Cunha, Michelle M A C Ribeiro, Rodrigo A A Muñoz, Eduardo M Richter
Paracetamol is an active ingredient commonly found in pharmaceutical formulations in combination with one of the following compounds: codeine, orphenadrine, promethazine, scopolamine, and tramadol. In this work, we propose a unique analytical method for determination of these active ingredients in pharmaceutical samples. The method is based on capillary electrophoresis with capacitively coupled contactless conductivity detection. The separation was achieved on a fused silica capillary (50 cm total length, 40 cm effective length, and 50 μm id) using an optimized background electrolyte composed of 20 mmol L(-1) β-alanine/4 mmol L(-1) sodium chloride/4 μmol L(-1) sodium hydroxide (pH = 9...
February 20, 2017: Journal of Separation Science
Tong Wang, Hai-Long Wu, Li-Xia Xie, Li Zhu, Zhi Liu, Xiao-Dong Sun, Rong Xiao, Ru-Qin Yu
In this work, a smart chemometrics-enhanced strategy, high-performance liquid chromatography and diode array detection coupled with second-order calibration method based on alternating trilinear decomposition algorithm was proposed to simultaneously quantify 12 polyphenols in different kinds of apple peel and pulp samples. The proposed strategy proved to be a powerful tool to solve the problems of co-elution, unknown interferences and chromatographic shifts in the process of high-performance liquid chromatography analysis, making it possible for the determination of 12 polyphenols in complex apple matrices within 10 min under simple conditions of elution...
February 20, 2017: Journal of Separation Science
Yelko Rodríguez-Carrasco, Juan Carlos Moltó, Jordi Mañes, Houda Berrada
Simple and highly efficient sample preparation procedures, namely, dispersive liquid-liquid microextraction and salting-out liquid-liquid extraction for the analysis of ten Fusarium mycotoxins and metabolites in human urine were compared. Various parameters affecting extraction efficiency were carefully evaluated. Under optimal extraction conditions, salting-out liquid-liquid extraction showed a better accuracy (84-96%) and precision (<14%) than dispersive liquid-liquid microextraction. Hence, a multi-biomarker method based on salting-out liquid-liquid extraction followed by gas chromatography with tandem mass spectrometry was proposed...
February 20, 2017: Journal of Separation Science
Yong-Qiang Liu, Hong Yu
A convenient and versatile method was developed for the separation and detection of alkaline earth metal ions by ion chromatography with indirect ultraviolet detection. The chromatographic separation of Mg(2+) , Ca(2+) and Sr(2+) was performed on a carboxylic acid base cation exchange column using imidazolium ionic liquid/acid as the mobile phase, in which the imidazolium ionic liquid acted as an ultraviolet-absorption reagent. The effects of imidazolium ionic liquids, detection wavelength, acids in the mobile phase and column temperature on the retention of Mg(2+) , Ca(2+) and Sr(2+) were investigated...
February 20, 2017: Journal of Separation Science
Shen Lin, Yingying Zhang, Wei Huang, Xiangchao Dong
In recent years, the efficient analysis of biological samples has become more important due to the advances of life science and pharmaceutical research and practice. Because biological sample pretreatment is the bottleneck for fast process, material development for efficient sample process in the high-performance liquid chromatography analysis is highly desirable. In this research, a cation-exchange restricted access monolithic column was synthesized by reversible addition-fragmentation chain transfer polymerization method...
February 20, 2017: Journal of Separation Science
Sheng-Xiang Gong, Xiao-Li Wang, Wei Liu, Ming-Lin Wang, Xia Wang, Zheng-Wu Wang, Ru-Song Zhao
Aminosilanized magnetic carbon microspheres as a novel adsorbent were designed and fabricated. And the adsorbent was used for the magnetic solid-phase extraction of bisphenols at trace levels from environmental water samples before liquid chromatography with tandem mass spectrometry analysis. The structure, surface and magnetic behavior of the as-prepared aminosilanized magnetic carbon microspheres were characterized by elemental analysis, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, powder X-ray diffraction, and vibrating sample magnetometry...
February 20, 2017: Journal of Separation Science
Hang Wang, Tongzhou Xu, Jiaojian Yuan
It is difficult to identify unknown impurities in nucleotide analogues by mass spectrometry because mass-spectrometry-incompatible mobile phases need to be used to separate the major ingredient from impurities. In this study, vidarabine monophosphate was selected, and unknown impurities were identified by online heart-cutting two-dimensional high performance liquid chromatography and linear ion trap mass spectrometry. The one dimensional reversed phase column was filled with a mobile phase containing non-volatile salt...
February 17, 2017: Journal of Separation Science
Xinhong Yu, Xu Ling, Li Zou, Zilin Chen
A novel polymeric monolith column with a β-cyclodextrins-graphene composite was prepared for extraction of methyl jasmonate. A simple, sensitive and effective polymeric monolith microextraction with high-performance liquid chromatography method has been presented for the determination. To carry out the best microextraction efficiency, several parameters such as sample flow rate, sample volume and sample pH value were systematically optimized. In addition, the method validation showed a wide linear range of 5-2000 ng mL(-) ¹, with a good linearity and the low limits of detection for methyl jasmonate...
February 16, 2017: Journal of Separation Science
Binnaz Demirci, Nilay Bereli, Sevgi Aslıyüce, Gözde Baydemir, Adil Denizli
The protein C imprinted monolithic cryogel was synthesized using 2-hydroxyethyl methacrylate by redox cryo-polymerization method. The prepared monolithic cryogel was characterized by Fourier transform infrared spectroscopy, swelling test, surface area measurements and scanning electron microscopy. The non-imprinted cryogel was prepared as well for control. Adsorption of protein C from aqueous solutions was investigated in a continuous mode and several parameters affecting adsorption performance were optimized...
February 14, 2017: Journal of Separation Science
Didi Ma, Lanping Yang, Bo Yan, Guoxiang Sun
The quality consistency of Yinqiaojiedu tablets was monitored by extracting their electrophoretic fingerprint and marker compound data which were obtained using capillary electrophoresis. To select the suitable background electrolyte, wing-shape method was proposed. A background electrolyte composed of 103.1 mM boric acid, 51.6 mM sodium borate, 9.8 mM disodium hydrogen phosphate, and 15.6 mM sodium dihydrogen phosphate was used to separate compounds. Under the optimized background electrolyte, the content of three marker compounds was determined in 25 Yinqiaojiedu tablet samples...
February 14, 2017: Journal of Separation Science
Piotr Luliński, Magdalena Bamburowicz-Klimkowska, Mariusz Dana, Dorota Maciejewska
This study presents a validated strategy for the determination of tryptamine in the presence of its competitors, which involves the molecularly imprinted solid-phase extractions combined with high-performance liquid chromatography coupled with fluorimetric detection Tryptamine-imprinted microscale sorbent was produced from 4-vinylbenzoic acid and ethylene glycol dimethacrylate in methanol by precipitation polymerization, and its imprinting factor was equal to 15.4 in static experiments or 18.6 in dynamic binding experiments...
February 14, 2017: Journal of Separation Science
Menghua Li, Caina Jiao, Xiumin Yang, Chun Wang, Qiuhua Wu, Zhi Wang
A new kind of magnetic N-doped mesoporous carbon was facilely prepared by one-step carbonizing a hybrid precursor (glucose, melamine and iron chloride) in a N2 atmosphere with eutectic salt (KCl/ZnCl2 ) as the porogen. The obtained magnetic N-doped mesoporous carbon showed excellent characteristics, such as strong magnetic response, high surface area, large pore volume, and abundant π-electron system, which endow it with a great potential as a magnetic solid phase extraction adsorbent. To evaluate its adsorption performance, the magnetic N-doped mesoporous carbon was used for the extraction of three phthalate esters from soft drink samples followed by high performance liquid chromatographic analysis...
February 13, 2017: Journal of Separation Science
Qiuying Li, Lili Lian, Xiyue Wang, Runnan Wang, Yuanyuan Tian, Xiaoyang Guo, Dawei Lou
Microcystins, produced by freshwater cyanobacteria, can be serious water pollutants, so it is important to monitor their concentration in drinking water. We have developed a method for rapid and accurate determination of microcystin levels in environmental water, using magnetic solid-phase extraction and high-performance liquid chromatography with UV detection. The magnetic composite material, which was combined with cetylpyridinium chloride, was prepared by hydrothermal synthesis. The optimal extraction of microcystins in water sample was achieved by optimizing the amount of adsorbent, the time of adsorption, the ratio of eluting solvent, and the volume of eluent...
February 13, 2017: Journal of Separation Science
Alireza Bazmandegan-Shamili, Ali Mohammad Haji Shabani, Shayessteh Dadfarnia, Masoud Rohani Moghadam, Mahboubeh Saeidi
A novel magnetic mesoporous silica material was synthesized and used as the sorbent for the magnetic solid-phase microextraction of diazinon and malathion before their quantification by high-performance liquid chromatography with UV detection. The sorbent was synthesized by a surfactant-templated one-pot sol-gel procedure using SiO2 -coated Fe3 O4 as the magnetic support, cetyltrimethylammonium bromide as the template and tetraethyl orthosilicate as the silicon source. The characteristics of the prepared sorbent were investigated using FTIR spectroscopy, scanning electron microscopy, and X-ray diffraction...
February 13, 2017: Journal of Separation Science
Yufeng Zhou, Haijiao Zheng, Jiutong Ma, Qiong Jia
In the present study, a novel poly(acrylamide-co-N-isopropylacrylamide-co-ethylene dimethacrylate) monolithic column modified with saline-modified delaminated layered double hydroxides was developed and exploited as the stationary phase in polymer monolith microextraction of β-agonists. Transmission electron microscopy, FTIR spectroscopy, scanning electron microscopy, X-ray photoelectron spectroscopy, and thermal gravimetric analysis with derivative thermogravimetric determination were employed to characterize the monoliths...
February 8, 2017: Journal of Separation Science
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