Current Analytical Chemistry
·
2024
·Vol. 21
·期 2
·124-133
·
IF 1.7
Zhengming Qian,Zhuobin He,Dongyin Lian,Qi Huang,Guoying Tan,Juying Xie
BackgroundFlavonoid is a type of active constituent in herbs and always used as the quality control markers of herbal medicines. Owing to the extensive diversity of flavonoids, numerous reference compounds are necessitated for the analysis of flavonoids, and some are usually very expensive, which engenders challenges in the analysis of flavonoids in herbal medicines. Consequently, the development of a simple, rapid, and reference compounds saving method is important for the determination of flavonoids in herbal medicines.ObjectiveIn order to develop a high-performance liquid chromatography (HPLC) method for the determination of 5 flavonoids (mangiferin, hesperidin, baicalin, buddleoside, and rutin) in five herbal medicines (Anemarrhenae rhizome, Sophorae flos, Citri reticulatae pericarpium, Scutellariae radix, and Chrysanthemi indici flos) with rutin.MethodsFive herbal medicine samples were prepared according to the Chinese Pharmacopoeia which includes ultrasound and reflux methods. The separation of the sample was performed on a PoroShell 120 EC-C18 (4.6 mm×100 mm, 2.7 μm) by gradient elution with 0.1% formic acid and acetonitrile at a flow rate of 1.0 mL/min. The wavelengths were set as follows: Anemarrhenae rhizome (363 nm), Sophorae flos (256 nm), Citri reticulatae pericarpium (236 nm), Scutellariae radix (263 nm), Chrysanthemi indici flos (354 nm).ResultsThe method validation showed that the established HPLC method was accurate and stable for quantitative analysis of flavonoids in five herbal medicines. The comparative analysis revealed that the determination results of the current HPLC method and Chinese Pharmacopoeia method are consistent, exhibiting less than 1% relative error. Remarkably, the developed HPLC method needs one cheapest reference compound (rutin) and costs 8 min for sample HPLC analysis.ConclusionThe developed HPLC method for quantitative analysis of five flavonoids in five herbal medicines is simple, rapid, and reference compound saving, which provides a good alternative method for quality control of flavonoids in herbal medicines.
研究领域:
药学
·
分析化学
✓ 已验证
DOI
高影响因子
MOLECULES
·
2022
·Vol. 27
·期 7
·2088
·
IF 4.927
Xue-Li Liu,Yong-Hui Wang,Shu-Yue Ren,Shuang Li,Yu Wang,Dian-Peng Han,Kang Qin,Yuan Peng,Tie Han,Zhi-Xian Gao,Jian-Zhong Cui,Huan-Ying Zhou
The efficient capture of multi-pollutant residues in food is vital for food safety monitoring. In this study, in-situ-fabricated magnetic MIL-53(Al) metal organic frameworks (MOFs), with good magnetic responsiveness, were synthesized and applied for the magnetic solid-phase extraction (MSPE) of chloramphenicol, bisphenol A, estradiol, and diethylstilbestrol. Terephthalic acid (H2BDC) organic ligands were pre-coupled on the surface of amino-Fe3O4composites (H2BDC@Fe3O4). Fe3O4@MIL-53(Al) MOF was fabricated by in-situ hydrothermal polymerization of H2BDC, Al (NO3)3, and H2BDC@Fe3O4. This approach highly increased the stability of the material. The magnetic Fe3O4@MIL-53(Al) MOF-based MSPE was combined with high-performance liquid chromatography-photo diode array detection, to establish a novel sensitive method for analyzing multi-pollutant residues in milk. This method showed good linear correlations, in the range of 0.05–5.00 μg/mL, with good reproducibility. The limit of detection was 0.004–0.108 μg/mL. The presented method was verified using a milk sample, spiked with four pollutants, which enabled high-throughput detection and the accuracies of 88.17–107.58% confirmed its applicability, in real sample analysis.Keywords:magnetic metal organic framework (MMOFs);magnetic solid-phase extraction (MSPE);multi-pollutants;high-performance liquid chromatography (HPLC)
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Analytical Methods
·
2018
·Vol. 10
·期 11
·1325-1330
·
IF 2.073
Yong Zhang,Zhizhong Zou,Guixing Chou
To quickly determine the amounts of kirenol, darutoside and darutigenol in Herba Siegesbeckiae using HPLC, the efficiency of sample cleanup with different solid phase extraction methods was systematically investigated. The results showed that a polymer based strong anion exchange (P-SAX, 200 mg/6 mL) sorbent could separate and enrich diterpenoids providing rapid determination without impurity interference. In this paper a new HPLC-UV method using a core–shell column (Boltimate C18 3.0 × 100 mm, 2.7 μm) for the quantitative determination of three diterpenoids was developed. Under optimum experimental conditions, P-SAX pretreatment with a core–shell analytical column exhibited satisfactory results in the determination of diterpenoids in Herba Siegesbeckiae with recovery rates of 95–102%, relative standard deviations below 1.1%, a limit of quantitation as low as 0.1 6 μg mL−1, and a short analytical runtime of 8 min. Finally, the proposed method was successfully applied in the profiling of diterpenoids in Herba Siegesbeckiae from different regions.
✓ 已验证
产品关联
DOI
高影响因子
Journal of Zhejiang University-SCIENCE B
·
2013
·Vol. 14
·期 7
·604-614
·
IF 1.108
Wang Shu-fang,Leng Jing,Xu Yi-min,Feng Mei-ling
Xiongdankaiming tablet (XDKMT), a well-known compound in traditional Chinese medicine, is widely used for the treatment of acute iridocyclitis and primary open-angle glaucoma. In this paper, accurate and reliable methods were developed for the identification of 20 constituents using high-performance liquid chromatography with photodiode array and electron spray ionization-mass spectrometry (HPLC-PDA/ESI-MS n ), and determination of nine of the constituents (chlorogenic acid, gentiopicroside, isochlorogenic acid B, diosmetin-7- O -β- d -glucopyranoside, apigenin, diosmetin, tauroursodeoxycholic acid, acacetin, and taurochenodeoxycholic acid) was developed using HPLC with ultraviolet absorption detector and evaporative light scattering detector (HPLC-UV/ELSD) for the first time. The best results were obtained on a Zorbax SB-C18 column with gradient elution using water (0.1% formic acid) (A) and methanol (0.1% formic acid) (B) at a flow rate of 0.7 ml/min. Tauroursodeoxycholic acid and taurochenodeoxycholic acid, owing to their low UV absorption, were detected by ELSD. The other seven compounds were analyzed by HPLC-UV with variable wavelengths. The calibration curves of all nine constituents showed good linear regression ( R
2 >0.9996) within the linearity ranges. The limits of detection and quantification were in the ranges of 0.0460–9.90 μg/ml and 0.115–24.8 μg/ml, respectively. The accuracy, in terms of recovery, varied from 95.3% to 104.9% with relative standard deviations (RSDs) less than 4.4%. Precision (with the intra- and inter-day variations less than 4.4%) was also suitable for its intended use. The developed method was successfully applied for the analysis of major components in XDKMT, which provides an appropriate method for the quality control of XDKMT.
研究领域:
中药学
·
分析化学
✓ 已验证
DOI
PubMed
高影响因子
NUCLEAR MEDICINE AND BIOLOGY
·
2026
·
IF 3.1
Lei Xu,Zhenhao Dong,Hong Zhang,Antonio Arleques Gomes,Wagner de Rossi,Jing Wang,Arian Pérez Nario,Qinggang He
A post-column derivatization high-performance liquid chromatography-ultraviolet (HPLC-UV) method was developed to determine Kryptofix 2.2.2 (K2.2.2) in PET tracers. This method utilizes the specific complexation between K2.2.2 and Pb 2+ , forming a stable 1:1 host-guest complex. The complexation produces a bathochromic shift in UV absorption maximum (from 210 nm to 254 nm), enabling sensitive detection. This approach addresses the limitations of poor performance and narrow applicability associated with direct single-method detection of K2.2.2. The chromatographic conditions were optimized (column flow rate: 0.7 mL·min −1 ; derivatization reagent flow rate: 0.7 mL·min −1 ; Pb 2+ concentration: 50 μg·mL −1 ) and the method was validated. The results exhibited excellent linearity (1–100 μg·mL −1 , r 2 > 0.999), high reproducibility (relative standard deviation (RSD) < 5%), and a low detection limit (0.5 μg·mL −1 ). The method successfully quantified K2.2.2 in [ 18 F]FDG, [ 18 F]AV45 and [ 18 F]DPA714, achieving spiked recoveries of 89%–105%. Additionally, the method remained unaffected by interference from common sample components such as sodium chloride and sodium ascorbate. This method provides a novel and efficient quality control tool for the simultaneous analysis of radiochemical purity and K2.2.2 content in diverse PET tracers.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
BMC Complementary Medicine and Therapies
·
2020
·Vol. 20
·期 1
·1-10
·
IF 0
Li Hong-Ying,Fang Jiang-Ji,Shen Hua-Dan,Zhang Xue-Qiong,Ding Xiao-Ping,Liu Jun-Feng
Background Quantitation analysis and chromatographic fingerprint of multi-components are frequently used to evaluate quality of herbal medicines but fail to reveal activity of the components. It is necessary to develop a rational approach of chromatography coupled with activity detection for quality assessment of herbal medicines. Methods An on-line HPLC-ultraviolet detection-2,2′-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) free radical scavenging (HPLC-UV-ABTS) method was developed to obtain the chromatographic fingerprints and ABTS +• inhibition profiles (active fingerprints) of Rehmanniae Radix (Dihuang) and Rehmannia Radix Praeparata (Shu Dihuang). Eighteen compounds showing ABTS +• inhibition activity were identified by HPLC-fourier-transform mass spectrometry (HPLC-FTMS). Verbascoside was used as a positive control to evaluate the total activities of the samples and the contribution rate of each compound. The similarities of the chromatographic and active fingerprints were estimated by the vectorial angle cosine method. Results The results showed that the HPLC-UV-ABTS method could efficiently detect antioxidant activity of the herbal medicine samples. The antioxidants were different between the two herbs and several new antioxidants were identified in Shu Dihuang. A function equation was generated in terms of the negative peak area (x) and the concentrations of verbascoside (y, μg/mL), y = 2E-07 × 4 - 8E-05 × 3 + 0.0079 × 2 + 0.5755x + 1.4754, R 2 = 1. Iridoid glycosides were identified as main antioxidants and showed their higher contributions to the total activity of the samples. The total contributions of the three main active components in the Dihuang and Shu Dihuang samples to the total activity, such as echinacoside, verbascoside and an unknown compound, were 39.2–58.1% and 55.9–69.4%, respectively. The potencies of the main active components in the Shu Dihuang samples were two to ten times those in the Dihuang samples. Similarity values for S12 in the chromatographic fingerprints and S03, S12 and P03 in the active fingerprints were less than 0.9. The three batches of samples might show their different quality with the other samples. Conclusions The results suggested that the combination of “quantity-effect” research strategy and the HPLC-UV-ABTS analysis method could comprehensively evaluate the active components and quality of Dihuang and Shu Dhuang.
✓ 已验证
产品关联
DOI
PubMed
JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Haixia Liu,Honghong Rao,Jinxin Guo,Baolan Lu,Yuyun Wang,Rongxi Zhu,Xinzhen Du
A layer-by-layer chemical bonding strategy was developed for fast in situ growth of bifunctional mesoporous covalent organic framework submicrospheres (COF SMSs) on the nickel-chromium alloy (Ni-Cr) fiber substrate via the ultrasound-assisted Schiff-base reaction for the first time. COF SMSs showed well-defined morphology, extraordinary high surface area (1211 m 2 · g −1 ) and narrow mesopore (2.50 nm) as well as excellent stability. Furthermore, the resulting Ni-Cr fiber presented outstanding adsorption capability and improved selectivity for bisphenols (BPs). Consequently, an attractive SPME-HPLC-UV approach with the Ni-Cr@Ni-Cr LDHs NSs@COF SMSs fiber was proposed for rapid preconcentration and sensitive determination of BPs. By optimizing adsorption parameters, the SPME-HPLC-UV method presented good linearity for five BPs in the ranges of 0.02–200 ng·mL −1 with coefficients of determination ( R 2 ) higher than 0.999. Limits of detection and limits of quantitation were obtained from 0.003 ng·mL −1 to 0.006 ng·mL −1 and from 0.010 to 0.019 ng·mL −1 , respectively. Moreover, the intra-day and inter-day precision expressed as relative standard deviations (RSDs) was 1.57–3.52 % and 2.65–4.38 % for the proposed method with a single fiber, respectively. RSDs of the proposed method with different duplicate fibers were 3.25–6.72 %. The proposed SPME-HPLC-UV method was available for efficient preconcentration and sensitive detection of five BPs from real water and milk samples. The relative recoveries at three spiking levels of BPs were achieved in the range of 80.00–118.8 % with RSDs below 7.81 %. In addition, the prepared fiber still exhibited satisfactory adsorption performance after 120 adsorption-desorption cycles.
研究领域:
分析化学
·
环境科学
·
材料科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MICROCHIMICA ACTA
·
2021
·Vol. 188
·期 2
·1-9
·
IF 5.833
Senosy Ibrahim Abdelhai,Zhang Xin-Zhong,Lu Zhi-Heng,Guan Xiao-Yu,Yang Zhong-Hua,Li Jian-Hong,Guo Hao-Ming,Abdelrahman Talat Mahmoud,Mmby Mohamed,Gbiliy Asmaa
Fe 3 O 4 @MIL-100 (Fe)/PEI are used for the first time as an adsorbent material for the extraction of pesticide residues (epoxiconazole, flusilazole, tebuconazole, and triadimefon) from food matrices. The adsorbent proposed (Fe 3 O 4 @MIL-100(Fe)/PEI) was characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), field emission scanning electron microscopy (FE-SEM), thermogravimetric (TG) analysis, and vibrating sample magnetometer (VSM) techniques to evaluate the properties of the sorbent. Then, the Fe 3 O 4 @MIL-100 (Fe)/PEI was employed for the quantification of the four triazole fungicides in fruits and vegetables (apple, orange, tomato, cabbage, and cucumber) using HPLC-UV for separation and detection. During the extraction process, the main parameters such as amount of adsorbent, extraction time, pH value, ionic strength, eluting solvent, and eluting volume were optimized. Under the optimum conditions, good linearity of this method was observed for all analytes, with correlation coefficients ( R 2 ) ≥ 0.9908. The limits of detection (LODs) ranged from 0.021–3.04 μg kg −1 . The extraction recoveries of the four triazole fungicides varied from 73.9 to 109.4% with relative standard deviations (RSD) in the range 0.5 to 6.2%. Compared with other MOFs, the modification of Fe 3 O 4 @MIL-100 (Fe) with PEI shows high efficient adsorption due to the combined benefits of MIL-100 (Fe) and PEI. The material is easily synthesized, has good stability, and is of low cost.
Graphical abstract
研究领域:
分析化学
·
食品安全
·
环境科学
✓ 已验证
DOI
高影响因子
FOOD CHEMISTRY
·
2023
·
IF 8.8
Li Gao,Piao Xu,Jiaoyan Ren
This work described a sensitive and economical HPLC-UV method with FDAA derivatization to simultaneously detect 36 D/ l -amino acids, which provides higher sensitivity and lower cost than other HPLC-based methods. It was validated for linearity range (8–1000 µmol/L), limits of detection (2.68–62.44 pmol/L), limits of quantification (2.93 to 208.13 pmol/L), intraday precision (0.30 % − 5.31 %), interday precision (1.96 % − 8.04 %) and accuracy (86.53 % − 121.46 %). This method was then applied in the determination of D/L- amino acids abundance in fermented and unfermented food materials and showed the characteristics of each type of foods. The method also demonstrated good performance in another application case for the discrimination of different types of food materials based on D/L- amino acids profile. It emphasizes the ability of the method to study the characteristics, distribution and abundance of d -amino acids in foods and their potential application in food quality control.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
TALANTA
·
2021
·
IF 6.057
Xin-Qiao He,Yuan-Yuan Cui,Xiao-Hui Lin,Cheng-Xiong Yang
Development of novel functionalized adsorbents for efficient magnetic solid phase extraction (MSPE) is essential for promoting their versatile applications in sample pretreatment. Herein, we report the fabrication of a new polyethyleneimine-600 decorated magnetic microporous organic network nanosphere (Fe 3 O 4 @MON-PEI 600 ) for effective MSPE of trace non-steroidal anti-inflammatory drugs (NSAIDs) from different water samples. The core-shelled Fe 3 O 4 @MON-PEI 600 integrates the synergistic effects of Fe 3 O 4 , MON and PEI 600 , providing facile and effective extraction to NSAIDs via multiple hydrogen bonding , π-π and hydrophobic interactions. The inner MON shell employs π-π and hydrophobic interaction sites and the outer PEI-600 coat acts as the hydrogen bonding doner/receptor, which affords good extraction performance for NSAIDs. Under optimal conditions, the Fe 3 O 4 @MON-PEI 600 -MSPE-HPLC-UV method gives wide linear range (0.14–400 μg L −1 ), low limits of detection (0.042–0.149 μg L −1 ), good precisions (intra-day and inter-day RSDs < 4.5%, n = 6), and large enrichment factors (97.0–98.2). Extraction mechanisms and selectivity of Fe 3 O 4 @MON-PEI 600 are evaluated in detail. Moreover, Fe 3 O 4 @MON-PEI 600 is successfully applied to enrich the trace NSAIDs in different water samples with the concentrations of 0.7 and 0.8 μg L −1 for 1-naphthylacetic acid, 0.5 and 0.1 μg L −1 for naproxen as well as 0.7 μg L −1 for ibuprofen , respectively. The developed method not only affords a novel and efficient magnetic adsorbent for NSAIDs in aqueous media at trace level, but also provides a new strategy for the rational design and synthesis of multiple functionalized MON composites in sample pretreatment.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
CHROMATOGRAPHIA
·
2013
·Vol. 76
·期 13
·735-745
·
IF 1.437
Peng Xi-Tian,Li Ze,Zhang Yi,Liu Tao,Yu Qiong-Wei,Feng Yu-Qi
A novel mixed-mode stationary phase (OAS) has been prepared by bonding n -octyl and aminopropyl groups with the surface of silica gel. The obtained OAS stationary phase was characterized by Fourier transform infrared spectroscopy, elemental analysis, zeta potential and ion-exchange capacity. The mixed-mode one-site and two-site retention models were used to quantitatively describe the retention mechanism of the OAS stationary phase using three strong acidic analytes. The results indicated that the two-site model is more suitable for the description of mechanism of OAS phase. Then the OAS stationary phase was applied to separate ten water- and fat-soluble vitamins in a single run; the separation is based on the hydrophobic and ionic interaction mechanisms. A method for the simultaneous determination of ten water- and fat-soluble vitamins in commercial multivitamin tablets by high performance liquid chromatography with ultraviolet detection was established and validated according to the stability, linearity, accuracy and precision. Finally, the validated method was used to analyze the content of ten vitamins in two commercial multivitamin tablets and the recoveries were in the range of 89.2–111.0 %, with RSDs <6.1 %, indicating the good reliability of the proposed method.
研究领域:
分析化学
·
药物分析
✓ 已验证
DOI
高影响因子
Food Analytical Methods
·
2026
·Vol. 19
·期 1
·60
·
IF 3
Hussain Aisha,Wu Jiapeng,Wen Jiaxi,Xiong Chaomei
Sudan dyes, a class of azo dyes, are genotoxic and carcinogenic to humans. However, they are still used illegally to color food products and spices due to their color fastness. In this study, multi-functionalized magnetic silica nanoparticles (C 18 /DVB/NVP(4:1)-Fe 3 O 4 @SiO 2 MNPs) were synthesized, and solid–liquid extraction (SLE) coupled with magnetic solid phase extraction (MSPE) was employed for the extraction and preconcentration of five Sudan dyes (Sudan I − IV, Sudan Red 7B), followed by high-performance liquid chromatography/ultraviolet spectroscopy (HPLC–UV) for their detection in powdered chili pepper samples. The SLE conditions for the analytes in powdered chili pepper samples were optimized. Under optimal conditions, the extraction recovery ranged between 78.0% and 106.9%. We investigated and optimized the potential factors that may affect the efficiency of MSPE. Under these optimal conditions, calibration curves showed good linearity ( R 2 > 0.9989) across the tested concentration range of 0.98 to 125 µg/g. The limits of detection for the five Sudan dyes were in the range of 0.06–0.26 µg/g. The intra-day and inter-day accuracy ranged from 93.5% to 106.3% with a relative standard deviation (RSD) of not more than 9.1%. The developed method was successfully applied to analyze ten different commercial brands of powdered chili pepper samples purchased from markets in Wuhan, confirming its feasibility for routine analysis of illegal Sudan dyes in these samples.
✓ 已验证
产品关联
DOI
高影响因子
危险品化学品经营许可证（带存储）