ANALYTICAL LETTERS
·
2025
·
IF 1.8
Wanying Zhao,Yanqin Chen,Jun Tan,Yanru Bai,Fudong Ma
A method utilizing high-performance liquid chromatography with evaporative light scattering detection (HPLC-ELSD) has been developed and validated for the simultaneous determination of raffinose, glucose, sucrose, and stachyose in waste liquid from cottonseed processing and in byproducts including cottonseed meal. The separation was performed using a carbohydrate ES column (250 × 4.6 mm, 5 μm) and isocratic elution with acetonitrile and water (70:30, v/v). The temperature of the column oven was maintained at 35 °C. The drift tube temperature for evaporative light scattering detection (ELSD) was operated 40 °C, while the nitrogen flow was set to 1.5 L·min−1. The saccharides were separated by HPLC-ELSD within 20 min. The coefficients of determination (R2 = 0.9986–0.9999) indicate that there was a linear relationship between saccharides and the response. The limits of detection were 0.004–0.023 mg·mL−1 and the quantification range was from 0.013 to 0.080 mg·mL−1. The intraday and interday precision were from 0.05 to 0.55% and 0.20 to 0.58%, respectively. The recovery was from 102.75 ± 2.03% to 106.76 ± 2.09% and the relative standard deviations were 1.87 to 1.98%. The method exhibited good stability in determining four saccharides in cottonseed processing waste liquid and the resultant byproduct cottonseed meal. This method exhibits high separation efficiency and sensitivity, excellent precision, and simplicity, which allows determination of the high value-added product, raffinose, in cottonseed processing waste liquid and meal.
研究领域:
食品科学
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分析化学
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产品关联
DOI
高影响因子
Analytical Methods
·
2025
·
IF 2.6
De-Huan Yang,Li-Lin Lin,Zhang-Feng Tang,Zengping Chen,Yao Chen,Tong Wang,Ruqin Yu
Lu'an Gua Pian tea (LAGP) is a traditional historical tea and one of the top ten famous teas in China. The price of LAGP from the same place of origin with different harvest time varies greatly in the market, among which the LAGP before the Qingming Festival (between April 4th and 6th every year) is regarded as a precious product. To accurately determine the harvest time of LAGP, especially around Qingming, HPLC-DAD combined with three different data analysis strategies (including targeted components analysis, non-targeted components analysis, and non-targeted fingerprint analysis) was evaluated and compared. Four machine learning algorithms are used to build the corresponding classification models, among which principal component analysis coupled with linear discriminant analysis (PCA-LDA), partial least squares discriminant analysis (PLS-DA) and K-nearest neighbors (K-NN) achieved more than 95% classification accuracy. In addition, the non-targeted component analysis can classify LAGP picking time to a much smaller extent with an accuracy of 100% for PLS-DA. The advantages and disadvantages of three data analysis strategies were compared. Regardless of the data analysis strategy used, the final classification accuracy was satisfactory. The corresponding data analysis strategy can be selected according to the specific experimental purpose. This work provides a variety of alternative solutions based on HPLC-DAD for identifying the picking time of Lu'an Gua Pian.
研究领域:
食品科学
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分析化学
✓ 已验证
DOI
PubMed
高影响因子
Analytical Methods
·
2018
·Vol. 10
·期 46
·5577-5588
·
IF 2.073
Qian Liu,Hai-Long Wu,Zhi Liu,Rong Xiao,Tong Wang,Yong Hu,Yu-Jie Ding,Ru-Qin Yu
A methodology for simultaneously measuring seventeen polyphenols in six Chinese raw propolis samples by using chemometrics-assisted high performance liquid chromatography-diode array detection (HPLC-DAD) was developed and validated. With the aid of a second-order calibration method based on an alternating trilinear decomposition (ATLD) algorithm, HPLC analysis was easily achieved within 16.5 min even in the presence of heavily overlapped peaks and unknown interferents. The average recoveries were in the range of 95.2% to 118.7% with standard deviation less than 7.0% for the selected raw propolis. Figures of merit including sensitivity (SEN), selectivity (SEL), root mean square errors of prediction (RMSEPs), etc. were calculated to validate the accuracy of the proposed method. For further confirmation, a multiple reaction monitoring (MRM) method based on LC-MS/MS was adopted. The paired F-test and t-test results showed that there was no significant difference between the MRM and the proposed method at the 95% confidence level, which indicated that the developed ATLD-assisted HPLC-DAD method is a suitable tool for the rapid analysis of Chinese raw propolis. Considering its advantages of simplicity, rapidity, precision and accuracy, it might also be extended as an alternative and available method for the quality monitoring of propolis raw material in the pharmaceutical industry.
研究领域:
分析化学
·
药学
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产品关联
DOI
高影响因子
Analytical Methods
·
2019
·Vol. 12
·期 2
·141-148
·
IF 2.378
Xue Ren,Man He,Beibei Chen,Bin Hu
Herein, magnetic porous organic polymers (MOPs) prepared via an azo coupling reaction in water under mild conditions are evaluated for the extraction of seven cardiovascular drugs, including xylocaine, metoprolol, mexiletine, labetalol, propranolol, carvedilol and propafenone, from human urine samples for the first time. The extraction mechanisms are assumed to be electrostatic interaction and π–π stacking. The MOPs exhibited fast adsorption/desorption time (13 min) and high enrichment factors (315–365-fold) for target analytes. Based on this, a method coupling magnetic solid phase extraction with HPLC-UV detection was developed for the analysis of cardiovascular drugs. Under the optimized conditions, the LODs (S/N = 3) were in the range of 0.06–0.57 μg L−1 with an RSD (n = 5) of 4.3–8.6%, and the linear range was 0.2–200 μg L−1 for propranolol, 2–200 μg L−1 for metoprolol, and 0.5–200 μg L−1 for the other five analytes. The developed method was applied for the analysis of cardiovascular drugs in urine samples with recoveries of 89.0–112%. In order to further evaluate the application potential of this method, real-time monitoring of metoprolol in urine samples collected from volunteers treated with metoprolol tablets was performed. The proposed method is simple, fast, and sensitive and has good potential in the monitoring of cardiovascular drugs in competitive sports and clinical analysis.
研究领域:
分析化学
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药理学
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产品关联
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2023
·
IF 3
Yutao Lou,Zhiyong Sun,Yitao Chai,Hui Qin,Qing Hu,Yujia Liu,Xiaowei Zheng,Ying Hu,Meihua Bao,Jinping Gu,Yiwen Zhang
Donafenib and sorafenib are small molecule chemotherapy drugs for the management of hepatocellular carcinoma, with donafenib being a deuterated derivative of sorafenib. To date, a high liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method that quantify donafenib, sorafenib, and their main metabolites has not yet been developed. The objective of this study was to establish a HPLC-MS/MS method for the simultaneous detection of donafenib, donafenib-N-oxide, sorafenib, and sorafenib-N-oxide and for the pharmacokinetic studies in rat. The extraction of all analytes was achieved by simple protein precipitation utilizing acetonitrile. The Waters XBridge C 18 column (2.1 × 100 mm, 3.5 µm) was selected, and the analytes could be efficiently separated and quantitated during a 2.8 min gradient elution procedure. The method was linear within the predefined quantification ranges and provided acceptable precision (%CV < 9.4%), reproducible extraction recovery (99.4%–111.5%), and low matrix effect (88.1%–98.6%). The hemolysis effect did not interfere with the quantification of all analytes, and similar results were obtained by changing the anticoagulant K 2 -EDTA to heparin or sodium citrate. Plasma pharmacokinetics revealed that the values of t 1/2 , C max , and AUC 0-t of donafenib were 1.4-, 6.2-, and 3.1-fold higher than those of sorafenib, respectively. In conclusion, the proposed bioassay was successfully applied to pharmacokinetic studies in rat after administration of donafenib and sorafenib. Our work not only improves the bioanalytical method for determining the plasma concentrations of donafenib, sorafenib, and their N-oxide metabolites, but also provides a scientific reference for clinical pharmacokinetic studies.
研究领域:
药物化学
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临床药理学
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分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Current Pharmaceutical Analysis
·
2023
·Vol. 19
·期 4
·330-344
·
IF 0.6
Xu Bingyong,Gao Jiarui,Tang Kaixian,Zhang Fengmei,Liu Shan,Su Weike,Wang Jian
Background: To control the quality of various butyl rubber closures and assess their applicability to cefamandole nafate, HPLC/ GC-MS methods were developed to qualitatively and quantitatively analyze the organic components in various types of butyl rubber closures and drug powder of
cefamandole nafate for injection, and migration of these components from rubber closures to drug also were studied. Materials and Methods: The chemical components in the rubber closures and corresponding drug were identified by GC-MS in full scan mode and NIST mass library. A GC-MS method
in SIM mode was established to quantitatively analyze siloxane compounds, aromatic hydrocarbons and saturated chain-hydrocarbons in rubber closures and drugs. An HPLC method was established to quantitatively analyze antioxidants and sulfides from rubber closures and drugs. The turbidity values
of powder for injection were measured by a turbidimeter. Further, the correlation between the content of organic components in the drug and the clarity of the solution was analyzed. Results: It was found that the chemical components were released from butyl rubber closures and migrated
to the drug, which influenced solution clarity of cefamandole nafate for injection and was the main factor to cause solution turbidity of powder for injection. The gradual migration of components occurred over time with the use of common butyl rubber closures, but the coated butyl rubber closures
(rubber plated with membrane) were coated with a polytetrafluoroethylene film to block the contact between rubber closures and the drug, and could effectively prevent the migration of the components from rubber closures to drugs. The organic components in the butyl rubber closures were mainly
identified as siloxanes, saturated chain-hydrocarbons, and antioxidants. An unknown ingredient was identified as 1-piperidinecarboxaldehyde, and trace amounts of toxic toluene were also detected within limits. Conclusion: It is suggested that rubber plated with membrane or rubber closures
of high quality were applicable to cefamandole nafate for injection and should be used in its production. HPLC/ GC-MS methods can be used as an effective method for quality control of butyl rubber closures and compatibility research with drugs to ensure drug safety for the public.
研究领域:
药学
·
分析化学
✓ 已验证
DOI
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2013
·Vol. 37
·期 5
·587-594
·
IF 2.591
Ting Yang,Chao Ma,Huaixia Chen,Yajie Zhang,Xueping Dang,Jianlin Huang
An IPC-imprinted (IPC is isoprocarb) poly(methacrylic acid)/SiO 2 hybrid monolithic column was prepared and applied for the recognition of the template. The hybrid monolithic column was synthesized in a micropipette tip using methyltrimethoxysilane as the inorganic precursor, 3-(methacryloxy)propyltrimethoxysilane as the coupling agent, and ethylene glycol dimethacrylate as the cross-linker. The synthesis conditions, including the porogenic solvent, coupling agent, volume ratio of the inorganic alcoholysate and organic part, were optimized. The prepared monolithic column was characterized by SEM and FTIR spectroscopy. A simple, rapid, and sensitive method for the determination of IPC in rice using the imprinted monolithic column microextraction combined with HPLC was developed. Several parameters affecting the sample pretreatment were investigated, including the eluent, washing solution, and loading sample volume. The linearity of the calibration curve was observed in the range of 9.0–1000 μg/kg for IPC in rice with the correlation coefficient ( r 2 ) of 0.9983. The LOD was 3.0 μg/kg (S/N = 3). The assay gave recovery values ranging from 91 to 107%. The proposed method has been successfully applied for the selective extraction and sensitive determination of IPC in rice and a satisfactory result was obtained.
研究领域:
分析化学
·
食品科学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
·
2023
·
IF 4.3
Jing-Yan Li,Qian Ge,Bin Liu,Zhen-Peng Gao,Chun-Feng Guo
This study aimed to develop a non-protein-based method for quantify cow milk in adulterated goat milk. The raw cow milk and raw goat milk samples were mixed separately with the same volume of cold acetone and centrifuged to remove their proteins. The supernatants were evaporated, and the residues were derivatized by silylation followed by GC-MS analysis. N-acetylglucosamine was identified as a thermostable non-protein biomarker of cow milk. Its concentration in the raw cow milk (146.7 mg/L) was 32 times higher than that in the raw goat milk. On this basis, a HPLC-MS/MS method using positive-ion electrospray ionization in parallel reaction monitoring mode was developed for quantifying cow milk in adulterated goat milk by determining peak area of the biomarker. The method showed good linearity over cow milk concentrations of 1–100% and could detect as low as 0.3% cow milk in adulterated goat milk. Besides, the method was characterized by a simple sample pretreatment process, rapid detection, high accuracy, and high precision. With this method, a sample could be analyzed in 10 min. The present study demonstrated the feasibility of quantifying cow milk in adulterated goat milk using N-acetylglucosamine as a biomarker of cow milk.
研究领域:
食品科学
·
分析化学
✓ 已验证
DOI
高影响因子
JOURNAL OF AOAC INTERNATIONAL
·
2020
·Vol. 104
·期 2
·479-484
·
IF 1.51
Lan Tao,Yu Congcong,Li Ren,Ma Zheng,Xi Xingjun,Chu Qiao
BackgroundSolanesol is an important pharmaceutical intermediate raw material, mainly used to synthesize coenzyme Q10, vitamin K2. It can be found prominent in potato stems and leaves. But now potato stems and leaves are always abandoned or discarded as they are not suitable for use as feed in aquaculture or other purposes. These agricultural waste resources can be reutilized as the corresponding extracts.ObjectiveTo develop a simple and standardized method for the detection of total solanesol in potato leaves and its extracts.MethodsN-hexane was chosen as the extraction solvent for three times in the solanesol extraction from potato leaves. HPLC-MS was used for the detection.ResultsThe LOQ was 0.3 µg/g and the linear range was from 0.1 to 50 µg/mL. The precision and stability were evaluated by the relative standard deviations (RSDs) of three samples (potato leaves, Extract-1, Extract-2) for interday and intraday. The accuracy of the method was evaluated by the recoveries of three different spiked concentrations of solanesol for three samples, and results showed it ranged from 80.7% to 99.0% with RSDs less than 8.7%.ConclusionsThe method we established can provide a simple and standardized way for the extraction and detection of total solanesol.HighlightsThe work laid a foundation for the resource reutilization of potato stem and leaf.
研究领域:
植物化学
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分析化学
·
药用植物学
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产品关联
DOI
PubMed
高影响因子
MICROCHIMICA ACTA
·
2018
·Vol. 185
·期 7
·1-8
·
IF 5.705
Wei Lanlan,Song Yuan,Liu Ping,Kang Xuejun
Polystyrene nanofibers were coated with copper nanoparticles (CuNPs) by a combination of electrospinning and in-situ reduction of Cu(II) using sodium borohydride as the reductant. The CuNPs on the nanofibers were characterized by energy dispersive spectrometry, scanning electron microscopy and transmission electron microscopy. A cartridge was packed with the nanofibers which then were activated with methanol and water. Glutathione (GSH) is found to quantitatively adsorbed by the packed cartridge at pH 3.0, and then can be desorbed with aqueous 2-mercaptoethanol and detected, after derivatization with ortho-phthalaldehyde, via high performance liquid chromatography with fluorometric detection. Under optimized conditions, the method has a 1.1 ng·mL −1 detection limit and a response that is linear in the 10–1000 ng·mL −1 GSH concentration range. The recoveries of GSH from artificial urine spiked at three levels (80, 400 and 800 ng·mL −1 ) are in the range of 94.6–98.6% with relative standard deviations (RSD) of <4.5% ( n = 5). The method was applied to assessing the differences in urinary GSH between high-risk infants and healthy infants. The results show that the levels of GSH of normal infants are significantly higher than those of high-risk infants ( P < 0.05).
Schematic of the preparation of CuNP-assembled nanofibers and the mechanism of extracting glutathione (GSH). GSH can be extracted by this material based on a strong interaction between the sorbent and GSH. This is attributed to the formation of Cu-S bonds between Cu and -SH.
研究领域:
分析化学
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生物医学
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产品关联
DOI
PubMed
高影响因子
MICROCHIMICA ACTA
·
2013
·Vol. 180
·期 11
·1109-1116
·
IF 3.434
Li Chenyu,Chen Ligang,Li Wei
We report on a method for the extraction of organophosphorus pesticides (OPPs) from water samples using mixed hemimicelles and magnetic titanium dioxide nanoparticles (Fe 3 O 4 @TiO 2 ) modified by cetyltrimethylammonium. Fe 3 O 4 @TiO 2 nanoparticles were synthesized by a hydrothermal process and then characterized by scanning electron microscopy and Fourier transform IR spectrometry. The effects of the quantity of surfactant, extraction time, desorption solvent, pH value, extraction volume and reuse of the sorbent were optimized with respect to the extraction of OPPs including chlorpyrifos, dimethoate, and trichlorfon. The extraction method was applied to analyze OPPs in environmental water using HPLC along with UV detection. The method has a wide linear range (100–15,000 ng L −1 ), good linearity ( r > 0.999), and low detection limits (26–30 ng L −1 ). The enrichment factor is ~1,000. The recoveries (at spiked levels of 100, 1,000 and 10,000 ng L −1 ) are in the range of 88.5–96.7 %, and the relative standard deviations range from 2.4 % to 8.7 %.
Schematic illustration of the preparation of CTAB coated Fe 3 O 4 @TiO 2 and its application as SPE sorbent for enriching OPPs
研究领域:
环境科学
·
分析化学
✓ 已验证
DOI
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.
研究领域:
中药学
·
分析化学
·
药理学
✓ 已验证
产品关联
DOI
PubMed
危险品化学品经营许可证（带存储）