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Journal of Environmental Sciences 2007年第10期19卷 1261-1265页

作者： hashi yuki WANG Tian-ran LI Yue-qi LIN Jin-ming State Key Laboratory of Environmental Chemistry and Ecotoxicology Research Center for Eco-Environmental Sciences Chinese Academy of Sciences Beifing 100085 China Shimadzu （Shanghai） Limited Beijing Office Analytical Application Center Beifing 100020 China

Seven polycyclic aromatic hydrocarbons （PAHs） in atmospheric particulates were determinated by high performance liquid chromatography （HPLC） with fluorescence detector using direction injection and an on-line enrichment trap column. The method simplified the sample pretreatment, saved time and increased the efficiency. With the on-line trap column, PAHs were separated availably even underground injecting 1.0 ml sample with relatively high column efficiency. The recoveries of the seven PAHs were from 85% to 120% for spiked atmospheric particulate sample. The limit of detection was 15.3-39.6 ng/L （S/N=3.3）. There were good linear correlations between the peak areas and concentrations of the seven kinds of PAHs in the range of 1-50 ng/ml with the correlation coefficients over 0.9970. Furthermore, it also indicated that the method is available to determine PAHs in atmospheric particulates well.

关键词： on-line enrichment on-line trap column high performance liquid chromatography (HPLC) atmospheric particulate polycyclic aromatic hydrocarbons (PAHs)

Analysis of keto-enol tautomers of curcumin by liquid chromatography/mass spectrometry

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Chinese Chemical Letters 2013年第8期24卷 685-687页

作者： Shin-ichi Kawano Yusuke Inohana yuki hashi Jin-Ming Lin Department of Chemistry Beijing Key Laboratory of Microanalytical Methods and InstrumentationTsinghua University Shimadzu Global COE for Application & Technical Development Shimadzu(China) Co.Ltd. Global Application Development Center Shimadzu Corporation Department of Chemistry Beijing Key Laboratory of Microanalytical Methods and Instrumentation.Tsinghua University

Keto-enol tautomers of curcumin were confirmed by reversed-phase liquid chromatography（RPLC）/ hybrid quadrupole ion trap/time-of-flight mass spectrometry（QIT/TOFMS）.Tautomers gave different MS/MS spectra in negative *** mass spectra were also obtained by hydrogen/deuterium exchange LC/MS/MS in positive *** results suggest that enol form is the major form in the solution（water/acetonitrile）.

关键词： Keto-enol tautomer Curcumin Liquid chromatography/mass spectrometry

Analysis of chloramphenicol in honey by on-line pretreatment liquid chromatography-tandem mass spectrometry

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Chinese Chemical Letters 2015年第1期26卷 36-38页

作者： Shin-ichi Kawano Hong-Yuan Hao yuki hashi Jin-Ming Lin Department of Chemistry Beijing Key Laboratory of Microanalytical Methods and InstrumentationTsinghua University Shimadzu Global COE for Application & Technical Development Shimadzu(China)Co.Ltd.

hloramphenicol is an antibiotic and one of the potential contaminants in ***-phase extraction is the key pretreatment procedure for analysis of chloramphenicol in *** this work,an on-line pretreatment liquid chromatography-tandem mass spectrometer system for sensitive,reliable and higher throughput analysis was *** the methylcellulose-immobilized reversed-phase column,sugars in a honey sample were efficiently removed in 1 *** a result,the limit of quantitation of chloramphenicol was 20 pg/mL（0.2 μg/kg honey）.

关键词： On-line pretreatment Liquid chromatography-mass spectrometry Chloramphenicol Honey

Construction of on-line supercritical fluid extraction with reverse phase liquid chromatography–tandem mass spectrometry for the determination of capsaicin

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Chinese Chemical Letters 2019年第1期30卷 99-102页

作者： Naoki Hamada yuki hashi Satoshi Yamaki Yanli Guo Lin Zhang Haifang Li Jin-Ming Lin Beijing Key Laboratory of Microanalytical Methods and Instrumentation MOE Key Laboratory of Bioorganic Phosphorous Chemistry & Chemical BiologyDepartment of Chemistry Tsinghua University China MS Center Shimadzu (China) Co. Beijing Branch

A novel on-line system composed of supercritical fluid extraction(SFE), dilution line and reverse phase liquid chromatography/mass spectrometry(RPLC/MS) was constructed for on-line extraction and reverse phase separation of some fat-soluble components in foods. Three columns including a trap column,concentration column and analytical column were used for trapping the fat-soluble components, on-line enrichment and reverse phase separation, respectively. Capsaicinoids were on-line extracted by a CO_2 supercritical fluid, then concentrated and separated by using the C_(18) columns, finally detected by mass spectrometry(MS). Capsaicin eluted at 10.1 min and limit of detection(LOD, S/N=3) for the standard solution is 0.55pg. The linearity was calculated with a value of coefficient of determination(R^2)≥0.998 in the range of 1.1–8.5 ng. Concentrations of capsaicin in the green, yellow, and red bell peppers were determined to be 60.33 ng/g, 31.79 ng/g, 35.38ng/g, respectively.

关键词： Supercritical fluid extraction Liquid chromatography-mass spectrometry Column-switching system Capsaicin

用在线样品预处理技术通过高效液相色谱测定血样中的药物

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色谱 2004年第4期22卷 313-315页

作者： hashi yuki 吕冬曹磊 Shimadzu (Hong Kong) Limited Beijing Office Analytical Applications Center Beijing 100020 China

The flow diagram of this on-line sample pretreatment system is shown in Fig.1.

关键词：血浆血清高效液相色谱在线预处理柱转换药物分析

Determination of phthalate esters in physiological saline solution by monolithic silica spin column extraction method

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Journal of Pharmaceutical Analysis 2011年第2期1卷 92-99页

作者： Lu Lu yuki hashi Zhi-Hua Wang Yuan Ma Jin- Ming Lin State Key Laboratory of Chemical Resource Engineering Beijing University of Chemical Technology Beijing 100029 China Department of Chemistry Tsinghua University Beijing 100084 China Shimadzu Global COE for Application & Technical Development Shanghai 200052 China

Monolithic silica spin column extraction （MonoSpin-SPE） was developed as a simple, sensitive, and eco-friendly pretreatment method which combined with ultra-fast liquid chromatography-mass spectrometry （UFLC-MS） to determine the levels of six phthalate esters, dimethyl- （DMP）, diethyl- （DEP）, dipropyl- [ DPrP], butyl-benzyl- （BBP）, dicyclohexyl- （DcHP）, and di-n-octyl-（DOP） phthalate in physiological saline samples. Under optimized experimental conditions, the method was linear in the following ranges： 0.2- 50 μg/L for DMP, DEP, DPrP, DcHP and DOP; 5- 100 μg/L for BBP. The correlation coefficients （R2 ） were in the range of 0. 9951 - 0. 9995 for all the analytes and the limits of detection （LODs） and limits of quantification （LOQs） were in the ranges of 0.02 - 0.9 μg/L and 0.08 - 2.7μg/L, respectively. The pretreatment process showed good reproducibility with inter-day and intra-day relative standard deviations （RSDs） below 8.5% and 11.2%, respectively. This method was used to determine the levels of six phthalate esters in physiological saline samples and the recoveries ranged from 71.2% to 107.3%. DMP and DEP were found in actual physical saline samples （brand A and brand B）.

关键词： monolithic silica spin column phthalate esters physiological saline samples ultra fast liquid chromatography- mass spectrometry (UFLC-MS)

FAST GAS CHROMATOGRAPHY APPLICATION TECHNIQUE

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FAST GAS CHROMATOGRAPHY APPLICATION TECHNIQUE

Profiling the metabolites of astrapterocarpan in rat hepatic 9000g supernatant

第四届国际华夏学者分析化学研讨会

作者： yuki hashi Analytical Center SHIMADZU CORP

Fast GC allows accurate and consistent analyses up to ten times faster than standard GC. Also have many features, such as higher resolution and less sample waste. Shimadzu’ s GC-2010 and GC-2014 systems have everything needed for fast GC, including: high pressure control unit, advance flow control unit, large split ratio, injector pressure program, fast temperature program, fast response detector and fast data acquisition rate of software. The capillary columns and experimental conditions were discussed. As a rapid growing analytical technique, more and more fast GC technique has been used for routine analysis. The applications for petrochemicals, pesticides and fragrances were described in detail. This paper provides an application of use fast GC technique for crude oil analysis.

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Chinese Journal of Natural Medicines 2019年第11期17卷 842-857页

作者： ZHANG Ya-Zhou XU Feng DONG Jing LIANG Jing hashi yuki LIU Guang-Xue LI Yao-Li SHANG Ming-Ying WANG Xuan CAI Shao-Qing State Key Laboratory of Natural and Biomimetic Drugs School of Pharmaceutical SciencesPeking UniversityBeijing 10000China School of Pharmaceutical Sciences Guizhou UniversityGuiyang 550000China Shimadzu China MS Center Beijing 10000China

Astrapterocarpan(AP) is a bioactive constituent of Astragali Radix and was selected as a model compound for investigating the in vitro metabolism of pterocarpans in this study. Its in vitro metabolism was conducted by incubation with rat hepatic 9000 g supernatant(S9) in the presence of an NADPH-generating system. At first, four compounds were isolated and their structures were elucidated as 6 a-hydroxy-AP(M1), astrametabolin I [M2, 1 a-hydroxy-9, 10-dimethoxy-pterocarp-1(2), 4-diene-3-one], 9-demethyl-AP(M3, nissolin) and 4-methoxy-astraisoflavan(M4, 7, 2’-dihydroxy-4, 3’, 4’-trimethoxy-isoflavan) on the basis of NMR data, respectively. Among them, M1, M2 and M4 were new compounds. Next, the metabolite profile of AP in rat hepatic S9 was obtained via HPLC-DAD-ESI-IT-TOF-MSn, and 40 new metabolites were tentatively identified. These newly identified metabolites included 9 monohydroxylated metabolites, 1 demethylated metabolite, 7 demethylated and monohydroxylated metabolites, 4 dihydroxylated metabolites, 1 hydration metabolite, 1 didemethylated metabolite, 2 glucosylated metabolites, 1 monohydroxylated and dehydrogenated metabolite, 2 monohydroxylated and demethylated and dehydrogenated metabolites, 2 dimerized metabolites, 3 dimerized and monohydroxylated metabolites, 2 dimerized and didemethylated metabolites, and 5 dimerized and demethylated metabolites. Finally, the major metabolic reactions of AP in rat hepatic S9 were summarized and found to be hydroxylation, demethylation, dimerization, hydration, and dehydrogenation. More importantly, the biotransformation from AP to M2 and the dimerization of AP by incubation with hepatic S9 were reported for the first time. In conclusion, this is the first report on the metabolism of a pure pterocarpan in animal tissues, and these findings will provide a solid basis for further studies on the metabolism of other pterocarpans.

关键词： Pterocarpan Astragali Radix LCMS Hepatic S9 Metabolism

Rapid Determination of Residual Quinolones in Honey Samples by Fast HPLC with an On-Line Sample Pretreatment System

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American Journal of Analytical Chemistry 2011年第2期2卷 200-205页

作者： Wei Du JianGuo Yao YueQi Li yuki hashi Shimadzu Corporation Kyoto Japan Shimadzu International Trading (Shanghai) Co. Limited Beijing China

A method of on-line pretreatment coupled to HPLC with fluorescence detection was developed and validated for the determination of nine quinolones in honey samples. This method simplified the complicated process of sample pretreatment and reduced sample treatment time. Recovery of the quinolones was between 92% - 101% for spiked honey samples. The limit of detection was 0.22 - 3.78 ng/mL (signal/noise ratio = 3). There was good linear correlation between HPLC peak area and concentration of the quinolones, with a linear range of 1.0 - 100.0 ng/mL and correlation coefficients >0.9997. The method proposed was validated for detecting quinolones in honey samples.

关键词： Antibiotics High Performance Liquid Chromatography (HPLC) Honey On-Line Pretreatment Quinolones

SIMULTANEOUS DETERMINATION OF CARBAMATE AND OGANOPHOSPHOUS PESTICIDES IN VEGETABLES AND FRUITS BY LIQUID CHROMATOGRAPHY-MASS SPECTROMETRY

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SIMULTANEOUS DETERMINATION OF CARBAMATE AND OGANOPHOSPHOUS P...