CHINESE JOURNAL OF CHEMISTRY
·
2011
·Vol. 29
·期 4
·778-782
·
IF 0.773
Haining Shi,Zonghua Wang,Hui Wang,Rui Zhao,Mingyu Ding
An anion-exchange chromatography method combined solid phase extraction (SPE) was developed for the simultaneous analysis of glycolate acid (GL), monochloroacetic acid (MCA) and dichloroacetic acid (DCA) in synthetical betaine products. The analytes and unknown anionic impurities were well separated on a Metrosep A supp5 anion-exchange column (150 mm×4 mm) with 2.0 mmol/L Na 2 CO 3 +2.0 mmol/L NaHCO 3 solution as eluent. Suppressed conductivity detection was used. A strong cation exchange (SCX) solid phase extraction (SPE) cartridge was used to reduce the concentration of matrix betaine and a Cleanert IC-Ag pretreatment cartridge was used to remove high Cl − concentration. The detection limits of GL, MCA and DCA were 0.09, 0.017 and 0.05 µg/L, respectively. The relative standard deviations (RSDs) of the retention times and peak areas were less than 0.09% and 0.49%, respectively. The recoveries of the three analytes were between 90.6% and 100.8%. The analytical results showed that GL and DCA were present in high concentration and no MCA was found when the proposed ion chromatography method was applied to three synthetical betaine samples. The proposed method is simple, sensitive and timesaving, and is also suitable for routine analysis in quality control of synthetical betaine products.
研究领域:
分析化学
·
药物质量控制
·
分离科学
·
环境分析
·
食品化学
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DOI
高影响因子
Horticultural Plant Journal
·
2017
·Vol. 3
·期 4
·165-171
·
IF 0
Yanhui ZHANG,Peiying LIU,Qianqian KONG,Shiyan XING,Xiaojing LIU,Limin SUN
Flavonoids and terpene trilactones, especially, ginkgo flavonglycosides, ginkgolides and bilobalides in leaves of ginkgo trees, need to be studied for effective application of these active components with high medical and health-care values. This study was aimed to provide scientific bases for genealogies selection and harvest season confirmation for Ginkgo biloba . A high-performance liquid chromatographic method (HPLC-ELSD) was developed to determine the contents of terpene trilactone and flavonoid of 36 ancient G. biloba genealogies from 19 provinces in China. The study indicated that the content gradually increased from April to August, and thereafter declined. Analysis of variance indicated that the contents of terpene trilactone, flavonoids, and their respective components had significant difference among 36 genealogies. The cluster analysis showed that No. 72 (Xing'an, Guangxi), No. 58 (Youyang, Chongqing), No. 82 (Rugao, Jiangsu), No. 123 (Huixian, Gansu), No. 99 (Dujun, Guizhou), No. 10 (Tai'an, Shandong) and No. 133 (Mentougou, Beijing) genealogies have higher content of terpene trilactone and flavonoid. These results can help us to select superior variety containing high content of terpene trilactone and flavonoid.
研究领域:
植物化学
·
药用植物学
·
天然产物化学
·
林木遗传育种
·
药物代谢
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DOI
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
·
2015
·Vol. 43
·期 10
·1569-1572
·
IF 0.754
Ming-Yan LUO,Bei LÜ,Guo-Bin SHEN,Fei-Fang ZHANG,Bing-Cheng YANG
Electrodialytic eluent generator, one of the key components of ion chromatography system, was fabricated and evaluated. The data achieved indicated that its performance could be comparable to that of commercial one. The maximal operation pressure was over 20 MPa, the generated KOH concentration was up to 100 mM, and the designed usage lifetime was about 354 day (take 8 h working time per day). This device will be helpful to the improvement of domestic instruments of ion chromatography.
研究领域:
分析化学
·
仪器科学与技术
·
分离科学
·
离子色谱技术
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DOI
高影响因子
MICROCHEMICAL JOURNAL
·
2014
·
IF 3.583
Shengling Sun,Jie Li
A method has been developed for the determination of zirconium (Zr), hafnium (Hf), niobium (Nb), tantalum (Ta), molybdenum (Mo), tungsten (W), and tin (Sn) in seawater by quadrupole inductively coupled plasma-mass spectrometry (Q-ICP-MS). The method is based on separation of the seven elements by extraction chromatography using N-benzoyl-N-phenylhydroxylamine (BPHA) supported on a microporous acrylic ester polymeric resin. The optimized procedure indicates that the BPHA resin has high selective adsorption for Zr, Nb, Mo, Sn, Hf, Ta, and W (known as fluoride soluble elements), whereas other interference and matrix elements are minimally adsorbed. The optimized eluent mixture with their molarity gives satisfactory recoveries for all analytes. The recovery can be achieved 99% for Zr, 97% for Nb, 97% for Mo, 99% for Sn, 99% for Hf, 95% for Ta, and 98% for W, respectively, by eluting with 6 mL of 6 mol L − 1 HF/1 mol L − 1 HCl. Furthermore, the technique for separation and enrichment of these elements provides a low total method blank. The detection limits for this method are 0.5 ppt for Zr, 0.2 ppt for Nb, 1.7 ppt for Mo, 1.0 ppt for Sn, 0.1 ppt for Hf, 0.1 ppt for Ta, and 0.3 ppt for W, respectively. The validity of the method is evaluated by replicate analyses of seawater reference materials; the precision of the results is better than 3% (RSD, n = 4), and the results are in good agreement with certified values. The established procedure has proved to be both practical and effective for seawater sample analyses.
研究领域:
分析化学
·
海洋化学
·
环境地球化学
·
痕量元素检测
·
质谱分析
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DOI
高影响因子
FOOD AND AGRICULTURAL IMMUNOLOGY
·
2019
·
IF 2.398
Lipeng Yuan,Bo Liu,Kaidan Yin,Zhen-Lin Xu
In this study, a heterologous competitive indirect enzyme-linked immunosorbent assay (ciELISA) for the determination of estriol (E3) in milk was developed. Rabbit polyclonal antibody specific for E3 was raised by introducing a carboxyl spacer arm from bromoacetic acid of E3 as immunizing hapten. A heterologous ciELISA using a coating hapten containing a carboxyl spacer arm from 6-ketoestriol of E3. The assay exhibited the required sensitivity for detection of E3 with limit of detection of 0.07 ng mL−1 and a working range from 0.41 ng mL−1 to 15.78 ng mL−1. Good recoveries were obtained ranging from 83.2% to 125.8% for E3 spiked milk samples. A satisfactory correlation (R2 = 0.994) between the results of ciELISA analysis and that of LC–MS/MS analysis indicated good accuracy and reproducibility of the proposed method, which was ideally suited as a rapid screening tool for routine E3 monitoring.
研究领域:
生物化学
·
分析化学
·
食品科学
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产品关联
DOI
高影响因子
TheScientificWorldJOURNAL
·
2014
·Vol. 2014
·期 1
·162465
·
IF 1.219
Haiying Luo,Yanping Xian,Xindong Guo,Donghui Luo,Yuluan Wu,Yujing Lu,Bao Yang
A new technique was established to identify eight organophosphate esters (OPEs) in this work. It utilised dispersive liquid-liquid microextraction in combination with ultrahigh performance liquid chromatography/tandem mass spectrometry. The type and volume of extraction solvents, dispersion agent, and amount of NaCl were optimized. The target analytes were detected in the range of 1.0–200 µ g/L with correlation coefficients ranging from 0.9982 to 0.9998, and the detection limits of the analytes were ranged from 0.02 to 0.07 µ g/L ( S / N = 3). The feasibility of this method was demonstrated by identifying OPEs in aqueous samples that exhibited spiked recoveries, which ranged between 48.7% and 58.3% for triethyl phosphate (TEP) as well as between 85.9% and 113% for the other OPEs. The precision was ranged from 3.2% to 9.3% ( n = 6), and the interprecision was ranged from 2.6% to 12.3% ( n = 5). Only 2 of the 12 selected samples were tested to be positive for OPEs, and the total concentrations of OPEs in them were 1.1 and 1.6 µ g/L, respectively. This method was confirmed to be simple, fast, and accurate for identifying OPEs in aqueous samples.
研究领域:
环境分析化学
·
污染生态学
·
毒物代谢
·
水质安全
·
持久性有机污染物
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DOI
高影响因子
Asian Journal of Pharmaceutical Sciences
·
2016
·Vol. 12
·期 2
·202-208
·
IF 0
Huiyan Shi,Chenzhi Hou,Liqiang Gu,Zhe Wei,Hang Xing,Meiyu Zhang,Shixiao Wang,Longshan Zhao,Kaishun Bi,Xiaohui Chen
The present study was designed to investigate the influence of the pretreatment of piperazine ferulate on pharmacokinetic parameters of methotrexate in methotrexate-induced renal injury rats. A simple and efficient high performance liquid chromatography coupled with mass spectrometry (HPLC-MS) method was developed to determine methotrexate in rat plasma. Methotrexate and syringic acid (internal standard) were extracted from rat plasma samples by protein precipitation with acetonitrile. The analysis was performed on a CAPCELL PAK C 18 column (150 mm × 4.6 mm, 5 µm) with acetonitrile and 5 mmol/l ammonium acetate aqueous (10:90, v/v ). The linear range was 5.0 × 10 −2 to 100.0 µg/ml for methotrexate. Other parameters were all within the acceptance criteria. The validated method was successfully applied the pharmacokinetic study of methotrexate between two methotrexate treated groups (with and without the pretreatment of piperazine ferulate). Compared with the methotrexate treated alone group, the pharmacokinetic parameters in the methotrexate with the pretreatment of piperazine ferulate group showed significantly lower MRT (0-t) , MRT (0-∞) and T 1/2 . Results suggested that methotrexate can be rapidly eliminated, cleared or metabolized in rat blood, which might be related to the pretreatment of piperazine ferulate. The method provided deeper insights into rational clinical use of methotrexate with the pretreatment of piperazine ferulate on cancer patients with renal dysfunction.
研究领域:
药理学
·
药物代谢
·
肾脏病学
·
肿瘤学
·
临床药学
·
分析化学
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DOI
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2013
·
IF 2.947
Chen Li,Feng Xu,Chen Cao,Ming-Ying Shang,Cui-Ying Zhang,Jie Yu,Guang-Xue Liu,Xuan Wang,Shao-Qing Cai
Traditional Chinese medicines (TCM) can be identified by experts according to their odors. However, the identification of these medicines is subjective and requires long-term experience. In this paper, electronic nose, headspace gas chromatography–mass spectrometry (GC–MS) and chemometrics methods were applied to differentiate two species of Asari Radix et Rhizoma by their odors. The samples used were the dried roots and rhizomes of Asarum heterotropoides var. mandshuricum (AH) and Asarum sieboldii (AS). The electronic nose was used to determine the odors of the samples and enabled rapid differentiation of AH and AS when coupled with principal component analysis. Headspace GC–MS was utilized to reveal the differences between the volatile constituents of AH and AS. In all, 54 volatile constituents were identified, and 9 major constituents (eucalyptol, eucarvone, 3,5-dimethoxytoluene, 3,4,5-trimethoxytoluene, methyleugenol, 2,3,5-trimethoxytoluene, croweacin, pentadecane and asaricin) could be used as chemical markers to distinguish these two species. AH contained higher relative contents of eucarvone (1.79–16.76%), 3,5-dimethoxytoluene (6.64–26.52%), 3,4,5-trimethoxytoluene/methyleugenol (6.43–31.67%) and 2,3,5-trimethoxytoluene (1.64–6.66%), whereas AS had higher relative contents of eucalyptol (14.06–24.95%), croweacin (5.64–13.55%), pentadecane (8.44–20.82%) and asaricin (7.03–13.45%). Moreover, AH and AS could be distinguished according to the contents of either all 54 identified volatile constituents or only the 9 major constituents by employing cluster analysis. The proposed method is rapid, simple, eco-friendly and can successfully differentiate these two species of Asari Radix et Rhizoma by their odors.
研究领域:
中药鉴定
·
分析化学
·
天然药物化学
·
代谢组学
·
药用植物学
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DOI
高影响因子
CHIRALITY
·
2012
·Vol. 24
·期 5
·391-399
·
IF 2.35
Hui Yu,Chenghua Yin,Cunyu Jia,Yu Jin,Yanxiong Ke,Xinmiao Liang
Two “click” binaphthyl chiral stationary phases were synthesized and evaluated by liquid chromatography. Their structures incorporate S-(−)-1,1'-binaphthyl moiety as the chiral selector and 1,2,3-triazole ring as the spacer. These chiral stationary phases (CSPs) allowed the efficient resolution for a wide range of racemic BINOL derivatives, particularly for nonpolar diether derivatives and 3-phenyl indolin-2-one analogs. The chromatographic data showed that the π–π interaction was crucial for enantiorecognition of these CSPs. Loss of enantioselectivity observed on CSP3 , which are lacking the triazole ring linkage, indicated that the triazole ring linkage took part in the enantioseparation process, although it was remote from the chiral selector of the CSP. The substitution of the phenyl group at 6 and 6' positions can significantly improve the separation ability of the CSP. The chiral recognition mechanism was also investigated by tracking the elution orders and studying the thermodynamic parameters. Chirality 24:391–399, 2012 . Copyright © 2012 Wiley Periodicals, Inc.
研究领域:
分析化学
·
药物化学
·
色谱学
·
手性分离
·
有机合成
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DOI
高影响因子
MARINE POLLUTION BULLETIN
·
2015
·Vol. 102
·期 1
·142-147
·
IF 2.991
Xiuping He,Xiaoqi Mei,Jiangtao Wang,Ziru Lian,Liju Tan,Wei Wu
An effective and highly selective molecularly imprinted material was prepared by suspension polymerization for the isolation and pre-concentration of synthetic estrogen diethylstilbestrol (DES) in seawater . The obtained MIPMs were proved to have more uniform size and porous structure, with maximum adsorption capacity of 8.43 mg g − 1 almost two times more than NIPMs (4.43 mg g − 1 ). The MIPMs showed no significant deterioration of the adsorption capacity after five rounds of regeneration. An off-line molecularly imprinted solid phase extraction (MISPE) method followed by HPLC–DAD was proposed for the detection of DES in seawater , and recoveries were satisfactorily higher than 77%. Four seawater samples in aquaculture area were analyzed and 0.61 ng mL − 1 DES was detected in one sample. The result demonstrated that this method can be used for the rapid separation and clean up of trace residual of DES in seawater.
研究领域:
环境分析化学
·
海洋环境污染
·
分子印迹技术
·
药物残留检测
·
水体污染物
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DOI
高影响因子
JOURNAL OF ANALYTICAL AND APPLIED PYROLYSIS
·
2020
·
IF 3.905
Yanshuxian Liu,Yilei Fan,Zhongping Huang,Huijun Liu,Lili Wang,Zhenlu Shen,Ichi Watanabe
A novel method based on on-line pyrolytic methylation-gas chromatography/mass spectrometry was established and applied into rapid determination of γ-hydroxybutyric acid (GHB) in human hair. With the pyrolytic methylation by tetramethylammonium hydroxide (TMAH), GHB was converted into its corresponding methyl ester in the pyrolyzer at 500 °C. Thus, GHB in hair samples could be well determined by GC/MS on a capillary column in SIM mode. To obtain optimum methylation conditions, important factors were investigated and then applied to the following experiments. The results were obtained as following: 500 °C as reaction temperature, 2:1 as the proportion of TMAH to GHB. The achieved calibration curve exhibited good linearity with the correlation coefficient of 0.9997 at the concentraion range of 2−200 ng/mg, and relative standard deviation (n = 3) from 1.3 %–7.7 %. The limit of detection and the limit of quantification were down to 0.3 ng/mg and 1.0 ng/mg, respectively. The precision ranged from 2.0 %–7.9 % and the recovery ranged from 98.5 %–107.4 %. The results of on-line pyrolytic methylation-GC/MS were in agreement with those observed by the referenced off-line silylation-GC/MS method. The method was applied to a real case of a woman addicted to GHB, the drug concentration in hair segments of 0−5 cm and 5−10 cm from the root strand well correlated with the use of GHB in different periods of her life. The proposed method demonstrated significant potential in the application of rapid determination for GHB in human hair.
研究领域:
法医毒理学
·
药物代谢
·
分析化学
·
生物样本分析
·
临床化学
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DOI
高影响因子
DALTON TRANSACTIONS
·
2022
·Vol. 52
·期 2
·376-383
·
IF 4.569
Enming Ping,Lingyun Kong,Mengyao Liu,Yunshan Zhou,Lijuan Zhang,Nan Chen
The reaction of porous γ-Al2O3 particles acting as both a sacrificial template and an aluminum source with 1,4-naphthalene diacid (H2NDC) resulted in the formation of γ-AlOOH@Al(OH)(1,4-NDC) composites, in which ZIF-67 was then loaded by the in situ crystallization method, leading to the formation of γ-AlOOH@Al(OH)(1,4-NDC)@ZIF-67 composites. The deliberately designed composite was used to separate H2/D2 at 77 K in a 1 m chromatographic column. The results demonstrated that the optimized composite can achieve the effective separation of H2/D2 in gas chromatography due to the additive effects of kinetic sieving and chemical affinity quantum sieving of Al(OH)(1,4-NDC) and ZIF-67. By optimizing chromatographic separation conditions, the resolution R reached 2.02 with the separation time t = 7.72 min. The composite also showed satisfactory repeatability and reproducibility.
研究领域:
材料科学
·
分离科学
·
物理化学
·
纳米材料
·
能源化学
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DOI
高影响因子
危险品化学品经营许可证（带存储）