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Food Analytical Methods · 2019 ·Vol. 13 ·期 3 ·718-725 · IF 2.413

HPTLC-Densitometry Determination of Riboflavin Fortified in Rice Noodle: Confirmed by SERS-Fingerprint

Chen Yisheng,Huang Caihong,Hellmann Bernhard,Xu Xueming

This paper presented a facile and efficient HPTLC method for quantifying riboflavin fortification in rice noodle that was a staple food popular in Asian countries. After high-throughput separation on silica gel plates with methanol/ethyl acetate/triethylamine (3/7/1, v /v/v) as the mobile phase, the obtained results were analyzed by fluorescence densitometry (mercury lamp, 360 nm excitation wavelength in combination with K400 optical filter). Quantification in this way offered high linearity ( R 2  = 0.9998 within 10–80 ng/band) and precision (RSD < 5.2%), adequate detectability (LOD = 0.1 and LOQ = 0.3 mg/kg), and accuracy (spike-recovery rates within 91.4–105.1%, RSD < 8.1%). While yielding good comparison to conventional HPLC detection, the developed quantification featured superiorly high efficiency. Apart from that, the separation results were further evaluated by SERS. By jointly using sodium borohydride reduced AgNPs as the active substrate and 633 nm incident laser wavelength, the developed HPTLC-SERS detection gave clear and sensitive fingerprint-like proof which enabled unambiguous confirmation by visual inspection. Balancing well between simplicity, detectability, efficiency, and reliability, the proposed method exemplarily shown the promising applicability of HPTLC as a versatile tool in food analysis.

CAS / MDL: 83-88-5
研究领域: 食品科学 · 分析化学
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Food Analytical Methods · 2018 ·Vol. 11 ·期 11 ·3170-3178 · IF 2.245

Screening of Phenolic Antioxidants in Edible Oils by HPTLC-DPPH Assay and MS Confirmation

Wang Liao,Chen Yisheng,Ye Zhiyang,Hellmann Bernhard,Xu Xueming,Jin Zhengyu,Ma Qinqin,Yang Na,Wu Fengfeng,Jin Yamei

The cytotoxicity of phenolic antioxidants had attracted marked attention, posing serious challenges to food safety. This paper presented a screening method for two major phenolic antioxidants (butylated hydroxytoluene and tert -butylhydroquinone) added in edible oils. To specifically visualize the targeted compounds after developing with toluene/ethyl acetate/methanol 8:1:1 ( v / v / v ) to 70 mm solvent front, the plate was subjected to a standardized 1,1-diphenyl-2-picrylhydrazyl assay. In addition to synoptical eye inspection, accurate quantification was realized by modified densitometric measurements: fluorescence mode, excitation wavelength 530 nm (D 2 and W lamp) without optical filter, which offered satisfactory sensitivity (8.5–17.5 mg/kg) and acceptable linearity ( R 2  > 0.999 within 50–200 ng/zone). Moreover, the established method was validated with edible oil samples, against EU Directive 2006/52/EC. Apart from that, the unambiguous confirmation of positive results was conveniently achieved by TLC-MS interface-mediated mass spectrometry. Featuring the merits of screening conception, the proposed method not only reached the goal of accurate quantification and conclusive identification of multi-phenolic antioxidants, but also excellently balanced the simplicity, detectability, and throughput of the screening workup. Therefore, it might be an attractive alternative to conventional methods.

CAS / MDL: 1948-33-0 128-37-0
研究领域: 食品安全 · 分析化学 · 营养学
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Chemistry Africa-A Journal of the Tunisian Chemical Society · 2022 ·Vol. 5 ·期 3 ·663-672 · IF 0

Microscopic and HPTLC Fingerprint Analysis a Tool for Authentication and Quality Control of Nelumbo nucifera

Maharana Subhashini,Mangaonkar Kiran,Phanse Manjusha

The demand for herbal raw material has increased and there is a requirement for quality control to look at the integrity of the herbal raw materials. There is a need for an easy and fast technique to check the quality and the authenticity of these raw materials. Nelumbo nucifera seeds have been used as traditional medicine for ages for curing various diseases. Its microscopy examination of fruit showed double-layered palisade tissue, rosette scleride, and epidermal pores. The morphology of starch grains were found to be simple, oval, and elliptical to polygonal in shape, which is the unique characteristic of the plant. Phytochemical analysis showed the presence of alkaloids, flavonoids, tannins, phenols, and saponin. A comparative study of cold and hot extraction of seed extract was carried out with respect to the HPTLC fingerprint profile. The HPTLC fingerprint of the cold and hot extract was done using butanol: water: acetic acid (4:1:1v/v/v) it showed the presence of 9 bands (R F 0.05–0.94) on the plate. The result shows that both cold and hot extract can be used for fingerprinting. Different concentrations of cold extract (100%, 80%, 50%, 20%) was used to standardize the lowest on plate concentration which can give maximum bands with high resolution, the results shows that a lower concentration of 50% can be used for the study. Thus, microscopy and HPTLC fingerprinting data along with morphological information can be used as a quality control tool to check the authenticity of the Nelumbo nucifera which has potential therapeutic value.

研究领域: 药用植物学 · 植物化学 · 中药质量控制
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FOOD CHEMISTRY · 2019 · IF 5.399

A new HPTLC platformed luminescent biosensor system for facile screening of captan residue in fruits

Yisheng Chen,Caihong Huang,Bernhard Hellmann,Zhengyu Jin,Xueming Xu,Guosheng Xiao

This study presented a HPTLC platformed luminescent biosensor system for screening captan residue. First, the potential bio-effects of layers materials on the detectability of a luminescent bacteria Photobacterium phosphoreum (ATCC 11040) as the sensor cell were assessed. From comparison, it was noteworthy that the combination of sensor cells with normal silica gel layer exclusively gave outstanding detectability (<10 ng/zone). On this basis, HPTLC mediated separation and biosensing was further optimized. Then, the obtained graphic results were digitally quantified via software processing, offering satisfactory selectivity, linearity ( R 2  = 0.9901 within 10–80 ng/zone) and sensitivity (0.5 mg/kg against MRLs ≥ 6 mg/kg). Additionally, the performance of the established method was validated with different fruits (recover rates 75–96%, RSD < 11.8%). Meanwhile, it was demonstrated that detectability of this hybrid system would be tuneable by altering the combination of bacteria strains and layer materials, which was meaningful to strengthen the usability of microbial biosensors.

CAS / MDL: 133-06-2
研究领域: 分析化学 · 环境科学 · 食品科学
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Food Chemistry-X · 2023 · IF 6.1

HPTLC + SRES screening of pesticide for point-of-care application as shown with thiram in juice

Zhijian Wang,Lixin Zhang,Yisheng Chen

In this study, a HPTLC-platformed SERS detection was established for screening thiram in juice. After a simple extraction, the sample liquid was separated on HPTLC plates, which resulted in a specific zone for the analyte. Following infiltration with atomize water, the band of interest was easily scraped off and eluted. In parallel, a flexible and SERS-active substrate was fabricated by the in-situ synthesis of gold nanoparticles within cotton fabrics. Under optimized conditions, fingerprint-like signal at 1376 cm −1 of the analyte were easily recorded by a hand-held Raman spectrometer with enough LOD (0.5 mg/L), LOQ (0.9 mg/L) and reproducibility (<11.7%). The optimized screening system was further validated with pear, apple and mango juice by determining the spike-and-recovery rates (75.6 to 112.8%). It was demonstrated that this method could be a facile point-of-care testing system tailored for pesticide screening.

CAS / MDL: 137-26-8
研究领域: 分析化学 · 环境科学 · 食品安全 · 即时检测
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PHYTOCHEMICAL ANALYSIS · 2025 · IF 2.6

HPTLC-Bioautography–MS-Guided Strategy for the Detection of Phthalides With Antimicrobial and Antioxidant Activities From Ligusticum chuanxiong Essential Oil

Zhijun Wang,Xiaomeng Tang,Lei Lv,Sicong Qiao,Mengxin Chen,Hongjie Song

Introduction Antimicrobial resistance and free radical-mediated oxidative stress and inflammation involved in many pathological processes have become treatment challenges. One strategy is to search for antimicrobial and antioxidant ingredients from natural aromatic plants. This study established a rapid and high-throughput effect-component analysis method to screen active ingredients from Ligusticum chuanxiong essential oil (CXEO). Objective The study aims to screen phthalides with antimicrobial and antioxidant activities from CXEO by high-performance thin-layer chromatography (HPTLC)-bioautography combined with HPLC-TOF/MS method. Methods Antimicrobial activity was evaluated by disc diffusion and micro broth dilution methods. Antioxidant capacity was performed by DPPH scavenging test. Phthalides in CXEO were identified using HPLC-TOF/MS method. HPTLC–bioautography technique was established to screen phthalides of antifungal and antioxidant activities. Results CXEO had significant inhibitory activity against Candida albicans , weak or undetected inhibitory activity against Staphylococcus aureus , Escherichia coli , and Pseudomonas aeruginosa . For tested strains of C. albicans , inhibition zone diameters ranged from 13 to 17 mm, and MICs were from 0.5 to 2 mg mL −1 . CXEO also had strong antioxidant activity, IC 50 value for scavenging DPPH free radicals was 1.014 ± 0.014 mg mL −1 . Nine phthalides in CXEO were tentatively identified. Ligustilide and senkyunolide A were screened to have both antimicrobial activity against C. albicans and strong DPPH scavenging property. Conclusion HPTLC-bioautography–MS-guided strategy is very practical for high-throughput screening of antifungal and antioxidant phthalides from CXEO. In vitro experiments have shown that phthalides and CXEO have good biological activities, which may be used to the treatment of C. albicans infection or oxidative stress damage caused by various diseases. The therapeutic potential should be validated in vivo in the future.

CAS / MDL: 551-08-6
研究领域: 药理学 · 植物化学 · 微生物学
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POLAR RESEARCH · 2018 · IF 1.5

Di(2-ethylhexyl) adipate (DEHA) detection in Antarctic krill (Euphasia superba Dana)

Xiangning Han,Daicheng Liu

In this reported study, a novel high-performance thin-layer chromatography (HPTLC) method was developed for the detection and quantification of the toxic substance di(2-ethylhexyl) adipate (DEHA) in Antarctic krill. This procedure was based on the extraction of DEHA by ultrasonic solvent extraction with anhydrous ethanol, silica-gel column chromatographic separation, HPTLC detection and quantification using petroleum ether/ethyl acetate/ acetone/glacial acetic acid (29:1:0.5:2d*, v/v/v/v) as the developing solvent and bromine thymol blue solution as the chromogenic agent. The content of DEHA in freeze-dried Antarctic krill was found to be ca. 0.63 ± 0.05 mg/g. The structure of DEHA in the Antarctic krill was subsequently determined by gas chromatography–mass spectrometry (GC-MS) and infrared chromatography, which verified the presence of this compound in the krill. The HPTLC method exhibited excellent accuracy, with a recovery of 97.1–101.6% and good precision with a relative standard deviation of 2.47–4.90%. The DEHA in Antarctic krill oil was extracted by n-hexane and detected using the same method described above, which verified that DEHA was also present in krill oil at a concentration of ca. 2.16 ± 0.08 mg/g. The presence of DEHA in kill oil is very concerning because of its demonstrated harmful ecotoxicity, and since Antarctic krill is the key link in the food chain in the Antarctic coastal marine ecosystem. The adverse effects of DEHA on Antarctic krill and the source of DEHA will be explored in future research.

CAS / MDL: 3710-84-7
研究领域: 环境科学 · 海洋生物学
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RSC Advances · 2022 ·Vol. 12 ·期 14 ·8317-8322 · IF 4.036

HPTLC screening of saccharin in beverages by densitometry quantification and SERS confirmation

Qifei Chen,Huaming Hou,Dan Zheng,Xueming Xu,Xingjun Xi,Yisheng Chen

As a widely used artificially synthesized sweetener, saccharin faced numerous disputes associated with food safety. Therefore, its fast analysis in food is of crucial importance. In this study, an analytical method for the fast and reliable screening of saccharin in various beverages was established and validated, by combining HPTLC with densitometry and surface enhanced Raman spectroscopy. The diluted sample liquid was directly sprayed and separated on a silica gel plate using a mixture of ethyl acetate and acetic acid in the ratio of 9 : 1 (v/v) as the mobile phase. The separation realized full isolation of the analyte from background noises. Then, a densitometry analysis in the absorption–reflection mode (working wavelength 230 nm) was optimized to obtain quantitative data, showing a good linearity in the range of 40–200 ng per band (R2 = 0.9988). The limits of detection and quantification were determined to be 6 and 20 ng per band, respectively, which were equal to 6 and 20 mg kg−1. The quantitative results also displayed satisfactory accuracy and precision, with a spike-recovery rate within 87.75–98.14% (RSD <5.13%). As a cost-efficient tool for confirmation, surface enhanced Raman spectroscopy was employed to profile the molecular fingerprint of the analyte eluted from the plate layer. Under optimized conditions (785 nm laser as the excitation light and silver nanoparticle loaded glass fiber paper as the active substrate), the elution of the saccharin band exhibited stable and sensitive surface enhanced Raman spectroscopy signals. This study demonstrated that HPTLC could be a versatile platform for food analysis, with outstanding simplicity and cost-efficiency.

CAS / MDL: 81-07-2
研究领域: 食品科学 · 分析化学
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MICROCHEMICAL JOURNAL · 2020 · IF 3.594

HPTLC-bioautography/SERS screening nifedipine adulteration in food supplement based on Ginkgo biloba

Yisheng Chen,Caihong Huang,Zhengyu Jin,Xueming Xu,Yina Cai,Yuxiang Bai

Ginkgo biloba was a popular phytomedicine as the essential ingredient of many food supplement. In this work, a bio-inspired HPTLC method was proposed for the visualized screening of nifedipine adulteration in food supplement based on Gingko biloba . To customize the visualization of the analyte by inhibiting bacterium ( Photobacterium phosphoreum ) bioluminescence, the silica gel plate that gives the highest detectability was selected as the stationary phase of separation. Thereafter, the HPTLC procedure (toluene and ethyl acetate 8/2, v/v, as the mobile phase, to a distance of 60 mm) was optimized and standardized as a sample cleanup tool to exclude noises caused by bioactive co-extracts. Then, the separation result fixed on the plate layer was selectively visualized as dark bands against the white background, only after 6 min exposure. To achieve quantitation of the obtained HPTLC images, an enhanced quantitative analysis was optimized via software (ImageJ) facilitated pixel scanning, offered remarkable sensitivity (LOD=24.0 μg/g), linearity ( R 2 =0.9985 within 50–300 ng/band) and precision (RSD<7.2%). Further, the developed method was validated with real samples (recovery rates within 81.0–92.8%). In conjunction with image quantitation, in-situ surface enhance Raman spectroscopy was incorporated into the analysis, using silver nanoparticles as the active substrate and He:Ne 633 nm lamp the incident laser source. The obtained SERS spectra displayed highly characteristic fingerprint patterns, enabling unambiguous confirmation of effect-directed results.

CAS / MDL: 8013-01-2 21829-25-4
研究领域: 药物分析 · 分析化学 · 食品科学 · 植物化学
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Food Analytical Methods · 2021 ·Vol. 14 ·期 4 ·814-822 · IF 3.366

HPTLC-Densitometry Screening and Mass Identification of Fluorescent Whitening Agents Contamination in Cereal Flour

Chen Yisheng,Huang Caihong,Xu Xueming

In recent years, there was increasing concerns on food safety issues associated with fluorescent whitening agents from package materials. Here, we reported the development of a facile and reliable method suitable for high-throughput quantification and identification of two common fluorescent whitening agents (FWA 184 and FWA 367) in cereal products (wheat and rice flour), platformed by high-performance thin-layer chromatography. First, the sample preparation and cleanup were rapidly accomplished via an optimized solid–liquid extraction. The extracts and reference standard were simultaneously separated on silica gel plates, using the mixture of toluene and ethyl acetate (10/0.3, v/v) as the mobile phase. Then, rapid quantification was performed with densitometry in fluorescent mode (365

CAS / MDL: 7128-64-5 5089-22-5
研究领域: 食品安全 · 分析化学
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Food Analytical Methods · 2018 ·Vol. 12 ·期 2 ·431-439 · IF 2.245

HPTLC Screening of Folic Acid in Food: In Situ Derivatization with Ozone-Induced Fluorescence

Wang Ping,Chen Yisheng,Xu Xueming,Hellmann Bernhard,Huang Caihong,Bai Yuxiang,Jin Zhengyu

This paper proposes a facile and specific method tailored for quantifying and confirming folic acid in food, based on the combination of high-performance thin layer chromatography with fluorescence densitometry and surface-enhanced Raman spectroscopy. Chromatography was carried out on silica gel plates, using methanol/ethyl acetate/ammonia (6:4:1, v / v / v ) as the mobile phase. For the first time, ozone gas was utilized as the derivative agent, which efficiently induced the appearance of strong fluorescence of the analyte. Thereafter, fluorescent densitometry measurements were carried out for quantitative purpose, offering good linearity ( R 2  > 0.999) and sensitivity (0.7–1.4 mg/kg). In addition, the applicability and reliability of the established method was validated with food and food supplement samples, showing good agreement with the data obtained by conventional HPLC-UV as the benchmark, but with remarkably higher efficiency. Apart from that, the in situ-obtained surface-enhanced Raman spectroscopic fingerprint of bands under optimized conditions (532-nm incident laser and tenfold concentrated silver nanoparticles) enabled unambiguous identification of the targeted compound, serving as a convenient and affordable tool to prevent potential mistake from false-positive results.

CAS / MDL: 59-30-3
研究领域: 分析化学 · 食品科学 · 生物化学
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Food Science and Human Wellness · 2024 · IF 5.6

Bio-screening and quantification of methyl paraben in vinegar and coconut juice separated by HPTLC

Yisheng Chen,Xingjun Xi

As a widely used food preservative, methyl paraben was experimentally evidenced with serious hormone-like adverse effects. Herein, a high performance thin-layer chromatography platformed bioluminescent bioautography and image analysis for the selective quantification and confirmation of methyl paraben was proposed and validated in vinegar and coconut juice. First, the detectability of the bioautography to the analyte on different layer materials was estimated, revealing that normal silica gel was the best choice. After that, the liquid of sample extract and working solution were separated to overcome the background noises due to co-extracted matrices. The separation result was then coupled to the optimized bioautography, enabling instant and straightforward screening of the targeted compound. For accurate quantification, bioluminescent inhibition pattern caused by the analyte was processed by image analysis, giving useful sensitivity (LOD > 16 mg/kg), precision (RSD < 10.1 %) and accuracy (spike-recovery rate 76.9 %–112.2 %). Finally, the suspected result was confirmed by determining its MS fingerprint, further strengthening the reliability of screening.

CAS / MDL: 7128-64-5
研究领域: 食品科学 · 分析化学 · 毒理学
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