JOURNAL OF COLLOID AND INTERFACE SCIENCE
·
2015
·
IF 3.368
Ling Zhu,Guanhong Xu,Fangdi Wei,Jing Yang,Qin Hu
A novel molecularly imprinted stir bar (MIP-SB) was developed with melamine (MA) as the template molecule in this study. The sorptive capacity of MIP-SB was nearly three times over that of non-imprinted stir bar (NIP-SB). The MIP-SB presented much better selectivity than NIP-SB when used to absorb MA and its analogues. An analytical method to determine MA in powdered milk was established by combining MIP-SB sorptive extraction with HPLC. The liner range was 0.0631–12.6 ng/mL with good correlation coefficient of 0.9983, and the limit of detection was 0.0127 ng/mL based on three times ratio of signal to noise. This method was successfully applied to the determination of MA in powdered milk with satisfactory results. The method built is simple and suitable for the determination of MA in milk products which is of great significance for quality control of milk products.
研究领域:
分析化学
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食品科学
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DOI
PubMed
高影响因子
Food Analytical Methods
·
2021
·Vol. 14
·期 11
·2420-2429
·
IF 3.366
Cao Jinping,Cheng Yuanzhi,Xu Bocheng,Wang Yizhen,Wang Fengqin
To ensure reasonable intake of selenium for humans and provide insights on the development and nutritional analysis of high-quality selenium-enriched food, we established a reliable and highly sensitive method for the determination of selenium species in Z0206 selenium-enriched polysaccharide (Se-EPS). By optimizing the pre-treatment conditions (different enzymes, enzyme combinations, enzymatic time, concentration of enzymes, and centrifugation time), we found that Se-EPS can be effectively hydrolyzed by proteinase K for 18 h, followed by HPLC-ICP-MS determination. The developed method presented high sensitivity with the limit of detection and quantitation in the range of 0.44–2.35 μg L −1 and 1.54–7.21 μg L −1 . The relative standard deviation (RSD) was all less than 10% and recovery was greater than 80% except for SeCys2, which further validated the repeatability and accuracy of the proposed method. Under the optimized conditions, we could determine 4 selenium species: elemental selenium (78.37%), seleno-methionine (14.27%), selenocystine (0.03%), and Se-methylselenocysteine (5.22%) in Se-EPS. This work provides new insights into the determination of different selenium species in selenium-enriched food.
研究领域:
分析化学
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营养科学
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食品科学
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DOI
高影响因子
Analytical Methods
·
2018
·Vol. 10
·期 41
·4978-4984
·
IF 2.073
Xing Huang,Kaipeng Zhang,Yanli Tong,Yongsheng Zhong,Zuanguang Chen
In this study, a gradient reverse phase high performance liquid chromatography combined with a capacitively coupled contactless conductivity detection (RP-HPLC-C4D) method for simultaneous determination of phospholipid and fatty glyceride in liposome was developed. After saponification, the fatty glyceride and two types of phospholipids were transformed into octanoic acid, palmitic acid and erucic acid, respectively, which were then separated and detected by RP-HPLC-C4D. The results showed good linearity in the range of 20–1000 μg mL−1 for octanoic acid and erucic acid and 10–1000 μg mL−1 for palmitic acid. The LODs of octanoic acid and palmitic acid reached 2.5 μg mL−1, and 10 μg mL−1 for erucic acid. The average recoveries of octanoic acid, palmitic acid and erucic acid were 100.2%, 102.9% and 101.4% (n = 9), respectively. The developed method could be effectively applied in the quality control and stability monitoring of liposome.
研究领域:
分析化学
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药剂学
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DOI
高影响因子
ANALYTICAL SCIENCES
·
2022
·Vol. 38
·期 1
·105-112
·
IF 1.967
Wu Xiaoxiao,Huang Jingjing,Zhang Chi,Kang Xuejun
A novel nanofiber-based solid phase extraction (NFSPE) coupled with HPLC–DAD was developed for the determination of salivary histidine, a new potential index of physiological events. The treatment of the sample was based on a coupling reaction of histidine with the diazotization products of sulfanilic acid and sodium nitrite in a slightly alkaline medium, followed by NFSPE. Nanofibers comprising polystyrene and zinc acetate were used as a novel solid-phase sorbent to extract derived histidine via the chelation of Zn 2+ with the imidazole group in the analyte. The eluted target compound was analyzed by HPLC–DAD. Good linearity was achieved with the concentrations of histidine ranging from 0.645 to 64.5 µM; the detection limit was 0.193 µM. The intra-day and inter-day coefficients of variation were less than 8.0%. The method was successfully applied to the determination of salivary histidine in the subjects exposed to a public speaking stress. Graphical abstract
研究领域:
分析化学
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生物医学
·
材料科学
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DOI
PubMed
高影响因子
Drug Research
·
2019
·Vol. 70
·期 01
·12-22
·
IF 0
Chaowei Zhang,Chengqun Han,Lili Sun,Jinlong Yu,Qiaogen Zou
Bepotastine besilate (here after referred to as BTST), chemically known as ({d(S)4[4[(4chlorophenyl) (2pyridyl) methoxy] piperidino} butyric acid monobenzene sulphonate), is a second-generation antihistamine drug. To the best of our knowledge, no studies concerning the isolation or identification of process-related impurities have been reported so far. The current study reports the development and validation of a stability-indicating RP-HPLC method for the separation and identification of 5 potential impurities in bepotastine besilate. In this experiment, the structures of 3 process-related impurities were found to be new compounds. They were characterized and confirmed by NMR and MS spectroscopy analyses. These 3 new compounds were proposed to be (S)-4-[(phenyl)-2-pyridinylmethoxy]-1-piperidinebutanoic acid,(Imp-A); 4-[(S)-(4-chlorophenyl)-2-pyridinylmethoxy]-1- piperidinebutyric acid, N-oxide (Imp-B) and (S)-4-[(4- chlorophenyl)-2-pyridinylmethoxy]-1-piperidylethane (Imp-C). In addition, an efficient optimized chromatographic method was performed on a Shimadzu Inertsil C8–3 column (150 mm×4.6 mm, 3 μm) to separate and quantify these 5 impurities. It was using 15 mmol ammonium formate buffer in water (pH adjusted to 3.8 with formic acid) and acetonitrile as the mobile phase in gradient mode. The method was developed to separate and quantify these 5 impurities obtained in the range of 0.05–0.75 μg/mL. It was validated and proven to be selective, accurate and precise and suitable. It is the first publication of identification and characterization data of the 3 new compounds. It is also the first effective HPLC method for separation and quantification of all of process-related impurities in bepotastine besilate.
研究领域:
药物化学
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分析化学
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DOI
PubMed
ANALYTICAL SCIENCES
·
2022
·Vol. 38
·期 7
·989-1002
·
IF 1.967
Zeng Qingli,Zhong Hui,Zhang Tianci,Huang Zhiqin,Li Laisheng
A large π-conjugated perylenediimide bridged bis (β-cyclodextrin)-bonded stationary phase (PBCDP) was first prepared and characterized. The chiral HPLC performance was systematically evaluated using a series of chiral probes. The results showed that PBCDP could resolve 36 kinds of chiral compounds in reversed-phase and polar organic modes with high resolutions ( R s) 1.48–3.28 for profens, 1.25–2.85 for triazoles, 1.34–5.29 for flavanones, 1.66–4.58 for amino acids and 1.22–1.97 for β-blockers. Especially, PBCDP could completely resolve acidic non-steroidal chiral drugs (profens) and simultaneously resolve basic five triazole pesticides, which were difficult to separate by ordinary CDCSP. Compared with CDCSP (15 kinds), the new stationary phase has a wider resolution range (36 kinds). Obviously, the synergistic inclusion of the two cavities of bridged cyclodextrin, as well as the large π–π stacking, hydrogen bond, dipole–dipole and basic primary amine site (–NH–) provided by the perylenediimide bridging group contributed together to the improvement of the above chiral separations. PBCDP was a new type of versatile chiral separation material without port derivatization. Graphical abstract
研究领域:
分析化学
·
色谱技术
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PubMed
高影响因子
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
·
2023
·
IF 4.3
Shouyin Wang,Shengjie Li,Wenhui Wang,Xiuxia Guo,Jinfeng Pan,Xiuping Dong
This paper aimed to develop a quantitative method based on high-performance liquid chromatography (HPLC) coupled with triple quadrupole tandem mass spectrometry (MS/MS) for the simultaneous determination of two protein carbonylation products derived from lysine residues in meat proteins, namely, α-aminoadipic semialdehyde (AAS) and lysinonorleucine (LNL). Mass spectrometry conditions and derivatization parameters were optimized and the linearity, repeatability, bias, the limit of detection (LOD), the lower limit of quantification (LLOQ), and recovery were validated. The developed method showed satisfactory linearity, repeatability, and sensitivity for both AAS and LNL. This method was applied to analyze the contents of these compounds in different meat products, and the formation of AAS was observed to be closely related to the severity of the manufacturing conditions. Moreover, AAS was demonstrated to be a reliable but more sensitive marker for protein carbonylation compared to the DNPH method, which could also provide information regarding the specific pathway of protein carbonylation.
研究领域:
食品科学
·
分析化学
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高影响因子
MICROCHIMICA ACTA
·
2015
·Vol. 183
·期 1
·415-421
·
IF 3.741
Liu Xingli,Wang Chun,Wu Qiuhua,Wang Zhi
Magnetic Fe 3 O 4 -doped porous carbon (MPC) was synthesized by using a metal-organic framework as a sacrificial template and iron salts as magnetic precursors. The textural properties of the MPC were characterized by scanning electron microscopy, transmission electron microscopy, X-ray diffraction, vibration sample magnetometry, and nitrogen absorption-desorption isotherms. The MPC possesses a high specific surface and is strongly magnetic. It was employed as an adsorbent for magnetic solid-phase extraction of four carbamates. The main parameters that affect extraction efficiency were investigated. The carbamates were analyzed by high performance liquid chromatography with ultraviolet detection at 208 nm. Under optimum conditions, good linearity was achieved for all analytes in the 1–100 ng g −1 concentration range, with correlation coefficients of > 0.9992. The limits of detection (at an S/N ratio of 3) are between 0.1 and 0.2 ng g −1 , and the recoveries of spiked samples ranged from 89.3 to 109.7 %.
A magnetic porous carbon (MPC) was synthesized using metal-organic framework as sacrificial template and Fe salts as magnetic precursor. The MPC showed high specific surface area and good magnetic property. It was employed as magnetic solid-phase extraction adsorbent for the extraction of carbamates from apple sample.
研究领域:
分析化学
·
环境科学
·
食品安全
·
材料科学
·
色谱技术
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DOI
高影响因子
MICROCHIMICA ACTA
·
2015
·Vol. 182
·期 9
·1791-1796
·
IF 3.741
Li Lu,Lin Zheng-zhong,Chen Xiao-mei,Zhang Hong-yuan,Lin Yi-dong,Lai Zhu-zhi,Huang Zhi-yong
Molecularly imprinted polymer (MIP) particles for malachite green (MG) were prepared by emulsion polymerization using methacrylic acid as the functional monomer, ethylene glycol dimethacrylate as the cross-linker, and a combination of Span-80 and Tween-80 as an emulsifier. The MIP particles were characterized by SEM micrographs and FT-IR spectra. Their binding capacity for MG was evaluated based on kinetic and isothermal adsorption experiments and compared to non-imprinted polymer particles. Analytical figures of merit include an adsorption equilibrium time of 15 min, an adsorption capacity of 1.9 mg∙g‾ 1 in acetonitrile-water (20:80), and an imprinting factor of 1.85. The MIP particles were successfully applied to the extraction of MG from fish samples spiked with MG and the other interfering substances prior to its determination of MG by HPLC. Spiked samples gave recoveries of MG that ranged from 86 to 104 %, much higher than that of the other interfering substance.
Molecularly imprinted polymer particles for malachite green (MG) were prepared by emulsion polymerization. They show adsorption capacity of 1.9 mg∙g‾¹ with imprinting factor of 1.85, and were successfully applied to the extraction of MG from spiked fish samples.
研究领域:
分析化学
·
环境科学
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DOI
高影响因子
Natural Product Communications
·
2023
·
IF 1.8
Wenjia Li,Qinggui Lei,Wenqing Li,Guoying Tan,Xingzhong Liu,Zhengming Qian
A high-performance liquid chromatography (HPLC) method for the determination of 4 nucleosides by one reference compound in Chinese cordyceps was developed. The sample of Chinese cordyceps was prepared by ultrasonic extraction with a 0.5% phosphoric acid aqueous solution. The separation of the sample was performed on a CORTECS T3 column (100 mm × 4.6 mm, 2.7 μm) by gradient elution with acetonitrile and water at a flow rate of 1.0 mL/min. The wavelengths were set as 258 nm (0-5 min), 252 nm (5-9.1 min), 258 nm (9.1-10.5 min), 249 nm (10.5-20 min) at which 4 nucleosides exhibited identical ultraviolet absorption. The accuracy, precision, reproducibility, and stability tests of the HPLC method were carried out, and the results indicated that the established HPLC method was suitable for the quantitative analysis of 4 nucleosides in Chinese cordyceps. This approach was compared to the traditional external standard method with 4 nucleoside reference compounds and the relative standard errors of the content determination results by the 2 methods were less than 3.5%. The HPLC method developed for quantitative measurement of 4 nucleosides in Chinese cordyceps is simple, lower cost, and time-saving, which provides a methodology alternative for quality control of Chinese cordyceps.
研究领域:
分析化学
·
药学
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DOI
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2012
·Vol. 35
·期 17
·2223-2227
·
IF 2.733
Rui Wang,Jianguang Luo,Lingyi Kong
Scutellaria baicalensis Georgi is a well-known medical plant widely used as a famous traditional Chinese medicine. It has been reported that S. baicalensis can protect against oxidative stress and possess anti-inflammatory effect. In the present paper, an HPLC-diode array-chemiluminescence detection method for on-line detection was successfully developed to screen antioxidants in complex S. baicalensis extracts. Using the proposed approach, eight compounds in the S. baicalensis extracts were found to possess a potential antioxidant activity. Furthermore, the effects of purified compounds on protecting RAW 264.7 cells from hydrogen peroxide injury were also investigated in vitro to confirm the established method, which were consistent with the results of HPLC-diode array-chemiluminescence detection method. These results demonstrated that this method was a useful technique for rapidly screening and identifying bioactive components from complex herbal medicines.
研究领域:
药理学
·
植物化学
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DOI
PubMed
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2013
·
IF 2.591
Sui Xiao,Li-Fang Zhang,Xu Zhang,Su-Mei Li,Fei-Qun Xue
Several Acalypha australis Linn. species are used in traditional medicine in Southeast Asia. In this work, the ultra-performance liquid chromatography/mass spectrometry fingerprints and the antibacterial activities of A. australis Linn. were investigated. An in-depth discussion on the reliability of identifying and obtaining potentially active compounds by spectrum-effect relationship and semi-preparative high performance liquid chromatography was conducted. The result shows that gallic acid and a compound with molecular weight of 634.1 in the fingerprints were the main antibacterial compounds. Compared to the crude extract of A. australis Linn., both compounds increase the antibacterial efficacy 10 to 20 times. Compounds with molecular weights of 154.0, 292.0, and 485.1 in the fingerprints were the auxiliary antibacterial compounds. Through the entire isolation procedure, we obtained these antibacterial compounds with purities of 92.53, 87.98, 90.73, 89.36, and 88.14%, respectively. This work provides a general model of the combination of ultra-performance liquid chromatography/mass spectrometry fingerprinting and antibacterial test to study the spectrum-effect relationships of A. australis Linn. This model can be used to discover further the active compounds of this herb.
研究领域:
药用植物学
·
天然产物化学
·
微生物学
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DOI
PubMed
高影响因子