著者
Maya KAMAO Yoshihisa HIROTA Yoshitomo SUHARA Naoko TSUGAWA Kimie NAKAGAWA Toshio OKANO Hiroshi HASEGAWA
出版者
The Japan Society for Analytical Chemistry
雑誌
Analytical Sciences (ISSN:09106340)
巻号頁・発行日
vol.33, no.7, pp.863-867, 2017-07-10 (Released:2017-07-10)
参考文献数
22
被引用文献数
6

This study aimed to develop a menadione (MD) determination method employing liquid chromatography–tandem mass spectrometry (LC-MS/MS) using a pseudo multiple reaction monitoring (MRM) technique, wherein two quadrupoles are used to monitor the same ion. Detection limits of 40 and 2 pg were obtained for MD and its deuterium-labeled form, respectively, whereas MD intra- and inter-assay coefficient of variation values were determined as 5.4 – 8.2%, with the corresponding recoveries equaling 90.5 – 109.6%. The developed method enables determination of MD in urine, plasma, cell extract, and culture media, demonstrating that pseudo multiple reaction monitoring can achieve quantification of compounds forming no suitable product ions, such as MD.
著者
Koji FURUKAWA Makoto HASHIMOTO Satoshi KANECO
出版者
(社)日本分析化学会
雑誌
Analytical Sciences (ISSN:09106340)
巻号頁・発行日
vol.33, no.10, pp.1189-1191, 2017-10-10 (Released:2017-10-10)
参考文献数
14
被引用文献数
4

A rapid determination of aniline in environmental water was examined based on liquid chromatography/tandem mass spectrometry (LC/MS/MS). Environmental water samples were diluted 20-fold with Mill-Q water and measured by LC/MS/MS after adding a surrogate substance (aniline-d5). In the results of the present study, the calibration curve of aniline showed good linearity in the range of 0.05 – 2.0 μg/L. Since the RSD (repeatability) by measuring repeatedly an aniline standard solution (0.05 μg/L, n = 7) was 3.2%, the repeatability of this work was very excellent. In addition, the recovery rate of aniline in environmental water was in the range of 99.0 – 102% with RSD 3.4 – 7.7%, and very good recovery test results were obtained. From these results, this analytical method was confirmed to be effective for aniline measurements of environmental water samples. Also, it is possible to conduct rapid analyses of aniline in environmental water without any solid-phase extraction process, compared to the solid-phase extraction-GC/MS method.
著者
Andrei BITA George Dan MOGOSANU Ludovic Everard BEJENARU Carmen Nicoleta OANCEA Cornelia BEJENARU Octavian CROITORU Gabriela RAU Johny NEAMTU Iulia Daria SCOREI Ion Romulus SCOREI John HUNTER Brad EVERS Boris NEMZER Florin ANGHELINA Otilia-Constantina ROGOVEANU
出版者
(社)日本分析化学会
雑誌
Analytical Sciences (ISSN:09106340)
巻号頁・発行日
vol.33, no.6, pp.743-746, 2017-06-10 (Released:2017-06-10)
参考文献数
20
被引用文献数
4

The paper describes a new, simple, selective and precise high-performance thin-layer chromatographic (HPTLC) method for the simultaneous identification and quantitative determination of boric acid (BA) and calcium fructoborate (CFB) in bulk and tablet/capsule dosage forms of dietary supplements. HPTLC silica gel G 60 F254 precoated glass plates were used as the stationary phase. The mobile phase consisted of 2-propanol–water 8:2 (v/v). The two boron-based compounds were adequately separated with the Rf values of 0.83 ± 0.01 (BA) and 0.59 ± 0.01 (CFB).
著者
Nobuyuki TAKAYAMA Lee Wah LIM Toyohide TAKEUCHI
出版者
(社)日本分析化学会
雑誌
Analytical Sciences (ISSN:09106340)
巻号頁・発行日
vol.33, no.5, pp.619-625, 2017-05-10 (Released:2017-05-10)
参考文献数
24
被引用文献数
12

The retention behavior of inorganic anions was studied in hydrophilic interaction chromatography (HILIC). In this study, five kinds of HILIC stationary phases (amino, imidazole, amide, pyridine and zwitterionic) were investigated. It was found that only amino and imidazole columns exhibited the separation of inorganic anions under HILIC conditions. The retention mechanism was further investigated under both columns. A reversed elution order of inorganic anions was observed under the HILIC condition compared with those observed under the ion-exchange chromatography mode (IEC). The effect of salt species and their concentration in the eluent were investigated under constant acetonitrile (ACN) content. Sodium chloride and sodium perchlorate were chosen as the salt, and the salt (sodium perchlorate) concentration was varied from 10 to 40 mM to confirm the effect of the electrostatic interaction. The slope values of the plots of the log retention factor (k) versus the log eluent concentration were calculated to be between –0.43 and –0.45 for the amino column, while those obtained on the imidazole column were between –0.68 and –0.73. Various concentrations of ACN were also examined with 20 mM sodium perchlorate, and the typical HILIC retention behavior was observed on both amino and imidazole columns. Due to the obtained results, it is considered that the separation of inorganic anions under the HILIC condition was achieved by both electrostatic interaction and partition.
著者
Shubo DONG Zhengyu YAN Hanyue YANG Zhen LONG
出版者
(社)日本分析化学会
雑誌
Analytical Sciences (ISSN:09106340)
巻号頁・発行日
vol.33, no.3, pp.293-298, 2017-03-10 (Released:2017-03-10)
参考文献数
40
被引用文献数
4

A sensitive non-derivatization method for the determination of the highly polar compound 3-aminopiperidine was developed using a mixed-mode column combined with a charged aerosol detector (CAD). Chromatographic conditions, including the type of detector, separation mode, and mobile phase composition, were optimized to achieve high sensitivity towards and sufficient retention of 3-aminopiperidine. Compared to the precolumn derivatization UV method, the current method showed higher recovery and greater simplicify. High sensitivity (LOQ <2.73 μg mL−1) and good precision (RSD of peak area <2%) were also observed in the current method. Furthermore, the parameters such as buffer solution and column bleed that affected the sensitivity of the CAD were investigated. Finally, the current method was applied for the determination of 3-aminopiperidine in linagliptin samples. This is a new non-derivative for the determination of 3-aminopiperidine, and constitutes a novel application of the CAD for the quantitative analysis of highly polar basic compounds.
著者
Tao YANG Fang ZHU Tianxiao ZHOU Jianzhong CAO Yibo XIE Meiyi ZHANG Yan WANG Dong-Sheng CAO Qinlu LIN Lin ZHANG
出版者
(社)日本分析化学会
雑誌
Analytical Sciences (ISSN:09106340)
巻号頁・発行日
vol.33, no.2, pp.191-196, 2017-02-10 (Released:2017-02-10)
参考文献数
43
被引用文献数
7

This study aimed to develop a label-free, sensitive, selective, and environment-friendly fluorescent peptide probe His-His-Trp-His (HHWH) for determining the concentration of copper ion (Cu2+) in aqueous solutions. The results demonstrated that the designed HHWH has a high selectivity and sensitivity for monitoring the concentration of free Cu2+ via quenching of the probe fluorescence upon a binding of Cu2+. The fluorescence intensity of the HHWH had a linear relationship with the concentration of Cu2+ between 10 nM and 10 μM, and the detection limit was 8 nM. Furthermore, HHWH could be regenerated with sulfide ions at least five times. The concentrations of Cu2+ in three different real water samples were detected using this probe, and the results were consistent with the one detected using an atomic absorption spectrometer. Thus, HHWH can be used as an accurate and feasible fluorescent peptide probe for detecting Cu2+ in aqueous solutions.
著者
Takahiro IWAI Koichi CHIBA Tomohiro NARUKAWA
出版者
(社)日本分析化学会
雑誌
Analytical Sciences (ISSN:09106340)
巻号頁・発行日
vol.32, no.9, pp.957-962, 2016-09-10 (Released:2016-09-10)
参考文献数
22
被引用文献数
11

The concentrations of arsenic (As) and cadmium (Cd) in the tobacco leaves, ash and smoke of 10 kinds of cigarettes collected from different countries worldwide were determined by ICP-MS after microwave-assisted digestion. Total As and Cd concentrations in the tobacco leaves ranged from 0.20 to 0.63 and 1.8 to 9.9 mg kg−1, respectively. By the speciation analysis of As in tobacco leaves and ash by HPLC-ICP-MS following acid extraction, arsenite [As(III)] and arsenate [As(V)] were determined and trace amounts of monomethylarsonic acid (MMAA), dimethylarsinic acid (DMAA), trimethylarsine oxide (TMAO), tetramethylarsonium (TeMA) and some unidentified As species were also found. Arsenic speciation for smoke absorbed in an aqueous solution was carried out. The sum of the As species in tobacco leaves, ash and smoke was in good agreement with the result of total As determination in each sample, and the recoveries of speciation were 100 ± 10%. The distributions and the behaviors of As species were clarified.
著者
Shuang-Qing ZHANG
出版者
(社)日本分析化学会
雑誌
Analytical Sciences (ISSN:09106340)
巻号頁・発行日
vol.32, no.6, pp.631-637, 2016-06-10 (Released:2016-06-10)
参考文献数
17
被引用文献数
7

Icaritin (ICT), a major component in herb Epimedium brevicornum Maxim., shows beneficial effects for the treatment of osteoporosis and various cancers, and is predominantly metabolized to glucuronidated icaritin (GICT). Although clinical trials of ICT have exhibited good safety and tolerance, the dynamic bioditributions of ICT and GICT have not been reported. In the present study, the chemical structure of GICT was firstly reported, and a reliable ultra-high performance liquid chromatography–tandem mass spectrometry method (UHPLC-MS/MS) was firstly established for the simultaneous quantifications of ICT and GICT in rat tissues. The dynamic distribution of ICT and GICT in rat tissues and their pharmacokinetic parameters have been reported for the first time. ICT, GICT and the internal standard coumestrol were separated on a C18 column with a gradient mobile phase of acetonitrile and water containing ammonium formate and formic acid at a flow rate of 0.3 mL min−1. The analytes were quantified by a triple quadrupole tandem mass spectrometer in the negative ionization mode. The lower limit of quantification values for ICT and GICT were 0.2 and 2 ng mL−1, respectively. Good selectivity, linearity, accuracy, precision and recovery were achieved, and no significant matrix effect was observed. The UHPLC-MS/MS was firstly applied to a dynamic biodistribution study of ICT and GICT in rats, following an intraperitoneal administration of ICT at a dose of 10 mg kg−1.
著者
Xiaozhen GUO Hao WU Shiwen GUO Yating SHI Juanli DU Panpan ZHU Liming DU
出版者
(社)日本分析化学会
雑誌
Analytical Sciences (ISSN:09106340)
巻号頁・発行日
vol.32, no.7, pp.763-768, 2016-07-10 (Released:2016-07-10)
参考文献数
32
被引用文献数
16

Polymeric ionic liquid-coated magnetic nanoparticles have been successfully prepared as adsorbents for the magnetic solid-phase extraction of four drugs, namely alfuzosin, doxazosin, terazosin and prazosin, from pharmaceutical preparations, urine samples and plasma samples. The four drugs were detected by fluorescence spectrophotometer. Several extraction parameters, including the pH of the solution; the type, ratio and volume of the desorbing reagent; the amount of adsorbent; the time of the extraction and desorption processes; and the addition of NaCl, were investigated and optimized. Linear responses were determined for the four drugs in the concentration range of 0.5 – 45 ng mL−1. The limit of detection values for alfuzosin, doxazosin, terazosin and prazosin, which were defined as three times the standard deviation of a blank sample, were determined to be 0.035, 0.034, 0.027 and 0.028 ng mL−1 (n = 11), respectively. Furthermore, this new method gave preconcentration factors of 114.5, 111.3, 111.1 and 108.5 for these four drugs.
著者
Weiwen HU Jian ZHANG Jinming KONG
出版者
(社)日本分析化学会
雑誌
Analytical Sciences (ISSN:09106340)
巻号頁・発行日
vol.32, no.5, pp.523-527, 2016-05-10 (Released:2016-05-10)
参考文献数
43
被引用文献数
4

Herein, we applied hypericin (Hyp) for the detection of DNA on streptavidin-functionalized magnetic beads (SA-MB) through non-covalent π-π stacking interaction between 1-pyrenebutanoic acid (PBA) and Hyp. Briefly, the target DNA (tDNA) was hybridized to morpholino oligonucleotide (MO) that was immobilized on the surface of SA-MB. PBA was incorporated to the backbone of tDNA by means of phosphate-zirconium-carboxylate coordination reaction. Then, fluorescent Hyp was linked to PBA via π-π stacking interaction. Under the optimal conditions, this biosensor displayed a good linear relationship between the fluorescence intensity and the tDNA concentrations in the range from 1 to 100 nM with a low detection limit of 2.9 nM. The mismatch type in a specific DNA sequence can also be efficiently discriminated. Compared with some other reports, this method is more convenient, and has great potential for practical applications.
著者
Hiroshi MORIWAKI Miho ISHITAKE Shusaku YOSHIKAWA Hidekazu MIYAKODA Jean-François ALARY
出版者
The Japan Society for Analytical Chemistry
雑誌
Analytical Sciences (ISSN:09106340)
巻号頁・発行日
vol.20, no.2, pp.375-377, 2004 (Released:2004-08-06)
参考文献数
13
被引用文献数
46 52

We describe a method for the simultaneous determination of 12 kinds of polycyclic aromatic hydrocarbons (PAHs) in sediment based on liquid chromatography-atmospheric pressure photoionization-mass spectrometry (LC/APPI/MS). The method consists of PAH extractions by ultrasonics, clean-up by a solid-phase extraction procedure and determination by LC/APPI/MS. The limits of the determination for PAHs in sediment using the proposed method ranged from 0.06 to 0.9 mg/kg. PAHs were detected by this method in sediment samples on the mg/kg level.
著者
Masaharu TANIMIZU Kazuya NAGAISHI Tsuyoshi ISHIKAWA
出版者
The Japan Society for Analytical Chemistry
雑誌
Analytical Sciences (ISSN:09106340)
巻号頁・発行日
vol.34, no.6, pp.667-674, 2018-06-10 (Released:2018-06-10)
参考文献数
29
被引用文献数
13 13

We developed a method for rapid and precise determination of B isotope ratios by MC-ICP-MS through an optimization of washout method, mass-discrimination correction and chemical separation. Resultant reproducibility of δ11B values was ±0.4‰ (2 × SD) when a simple standard-sample bracketing technique was used, and it was improved to be better than ±0.2‰ by a mass discrimination correction with a 7Li/6Li isotopic reference. A mixed solution, which consists of HNO3–HF–mannitol, allowed a rapid washout of B memory in the sample introduction line. The validation of this technique to a wide range of δ11B value and various B signal intensities was confirmed from a series of B reference solutions with δ11B values of –20 to +40‰ and 25 to 125 ng/g B. Analyses of seawater standard (BCR-403) and carbonate standard (JCp-1) with sample sizes of less than 50 ng B gave δ11B values consistent with those determined by TIMS as Cs2BO2+. The simple and high-precision technique developed here is applicable to various types of commercially supplied multiple collector ICP mass spectrometers without any modification of the sample introduction system from their original instrumental setting.
著者
Hiroshi SHIIGI Takahiro FUJITA Xueling SHAN Masahiro TERABE Atsushi MIHASHI Yojiro YAMAMOTO Tsutomu NAGAOKA
出版者
The Japan Society for Analytical Chemistry
雑誌
Analytical Sciences (ISSN:09106340)
巻号頁・発行日
vol.32, no.3, pp.281-285, 2016-03-10 (Released:2016-03-10)
参考文献数
20
被引用文献数
5 6

Generally, the characterization of a metal layer formed on a planar substrate has been achieved using scanning electron microscopy and transmission electron microscopy. These techniques provide details of the surface and/or the cross-section of a planar structure with high resolution. However, the evaluation of sphere-like structures is troublesome owing to the necessity to observe a sample from various angles and/or to calculate the yield from many values obtained for many samples, since the conventional methods can observe a sample only from one direction. We have developed a simple evaluation method for a thin metal layer on plastic microbeads based on its light-scattering properties using dark-field microscopy coupled with a spectrometer. The light-scattering intensity of gold-nanoparticle-coated microbeads depends significantly on the gold coverage. We believe that our study is significant because it describes the development and evaluation of the surface coverage of a thin metal layer on a sphere-like microstructure.
著者
Toshihiro OOMORI Takumi OKA Tooru INUTA Yoji ARATA
出版者
The Japan Society for Analytical Chemistry
雑誌
Analytical Sciences (ISSN:09106340)
巻号頁・発行日
vol.16, no.4, pp.365-369, 2000 (Released:2005-04-15)
参考文献数
12
被引用文献数
74 86

Acidic electrolyzed water (acidic EW), which is prepared by the electrolysis of an aqueous NaCl solution, has recently become of great importance for disinfection in a variety of fields, including medicine, the food industry and agriculture. In a previous paper we showed that: 1) acidic EW is a mixture of hypocholorite ion, hypochlorous acid and chlorine, depending upon the pH; 2) hypochlorous acid is primarily responsible for disinfection in the case of Escherichia coli K12 and Bacillus subtilis PCI219, both in clean culture media. In practice, however, the use of acidic EW is in many cases severely hampered due to the presence of a variety of non-selective reducing agents. In view of the salient nature of acidic EW, it is therefore strongly urged to establish an optimum way to use acidic EW in a variety of systems. The present paper is the first report on our attempt along this line in order to characterize the nature of the chemical changes that the bactericidal activity of the acidic EW deteriorates in the presence of organic materials, which include amino acids and proteins.
著者
Ikuma KURODA Yukihiro SHINTANI Masanori MOTOKAWA Shuzo ABE Masahiro FURUNO
出版者
The Japan Society for Analytical Chemistry
雑誌
Analytical Sciences (ISSN:09106340)
巻号頁・発行日
vol.20, no.9, pp.1313-1319, 2004 (Released:2005-01-21)
参考文献数
14
被引用文献数
80 93

A methodology of phosphopeptide-selective analysis coupled with column-switching HPLC utilizing titania as precolumn media is presented. Phosphopeptides were selectively enriched on titania packing within a protein/peptide mixture without any additional procedure, and analyzed by column-switching high-performance liquid chromatography. First, phospho-compounds were separated from complex mixtures by trapping them under acidic conditions on a titania packing, where non-phosphorylated compounds were effused out of the precolumn. Subsequently, phospho-compounds were desorbed from the titania column under a specific condition and analyzed. The behavior of phospho-compounds on a titania surface, especially adsorption/desorption, was precisely examined and optimized. A phosphoric buffer was successively employed for the elution of phosphopeptides on a titania surface by competition with the free phosphate group. From the successes of a selective concentration/analysis of phosphopeptides with column-switching HPLC with a titania precolumn, a novel phosphopeptide-selective RP-HPLC analysis has been shown to have an application possibility as a tool for phosphoproteomics.
著者
Ting-Ting HU Chun-Mei LU Han LI Zai-Xiao ZHANG Yun-Hui ZHAO Juan LI
出版者
The Japan Society for Analytical Chemistry
雑誌
Analytical Sciences (ISSN:09106340)
巻号頁・発行日
vol.33, no.9, pp.1027-1032, 2017-09-10 (Released:2017-09-10)
参考文献数
28
被引用文献数
11 18

The overuse of organophosphorus pesticides on cotton production is a big concern in China today. Therefore, developing methods for the rapid screening and confirming of pesticide residues in textiles has become a top public health security priority. Here, a method was established for the rapid screening and quantifying of 11 kinds of organophosphorus pesticides (ethoprophos, coumaphos, profenofos, diazinon, ethion, parathion, phosalone, quinalphos, dicrotophos, azinphos methyl, and tribuphos) in textiles by high-performance liquid chromatography high-resolution mass spectrometry (HPLC-HRMS). Rapid screening and quantifying could be completed by using software of Peakview and MultiQuant. Samples were extracted by the method of modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) and analyzed in the positive mode with MS detection. The results showed that the limits of detection were between 0.1 and 5.0 ng g−1, with correlation coefficients above 0.9990. The recoveries were in the range of 70.3 – 109.8%, with relative standard deviations from 5.1 to 16.4%. This method is accurate and simple, which can be used in the rapid screening and quantitative analysis of 11 kinds of organophosphorus pesticides in textiles.
著者
Takumi TAKANO Chiaki AOYAMA Yoshiro TERASAKI Kenichi SUZUKI Aki ANDO Yanting SONG Makoto TSUNODA
出版者
The Japan Society for Analytical Chemistry
雑誌
Analytical Sciences (ISSN:09106340)
巻号頁・発行日
vol.37, no.12, pp.1811-1814, 2021-12-10 (Released:2021-12-10)
参考文献数
15
被引用文献数
1

Therapeutic oligonucleotides have recently been approved in the United States, the EU, and Japan. Hence, the analysis of oligonucleotides is an important topic in drug development. Liquid chromatographic techniques are commonly used for purity verification and the determination of oligonucleotides. In ion-pair reversed-phase separation, several parameters, such as the pore size of the stationary phase, mobile phase additives, and column temperature, were investigated using three types of oligonucleotides (18, 19, and 20 mer). All of the investigated parameters could influence the separation, and they are expected to be useful for optimizing oligonucleotide separation.