最新刊期
卷 43 ， 期 7 ， 2024
- 摘要：This paper carried out the content determination and fingerprinting study of the hypoglycemic and uric acid-lowering active parts of Cyclocarya paliurus.（C. paliurus.），and evaluated the quality of C. paliurus. herbs from different origins. Under the guidance of activity screening，the extraction conditions were optimized. Using 30% ethanol aqueous solution as extraction solvent，a solid-liquid ratio of 1∶10，and ultrasonic extraction for 1 hour can extract the active part effectively. A high performance liquid chromatography（HPLC） method was used for the determination of the contents of chlorogenic acid，quercetin-3-O-β-D-glucuronide，quercitrin，kaempferol-3-O-β-D-glucuronide，isochlorogenic acid C and afzelin in the active part of C. paliurus.. Quality evaluation was based on the content variation of each ingredients with the origin. Among them，the Jiangxi herb S1 had the low content，which differed from the herbs of other origins. At the same time，a fingerprint of the active part of C. paliurus. was established. The similarity of the 10 batches of herbs was all greater than 0.9. PCA analysis showed that the quality differences of Jiangxi herb S1，Hunan herbs S6 and S8 were large. The inhibitory activities of α-glucosidase and xanthine oxidase showed that Hunan herb S5 had the best hypoglycemic and uric acid-lowering activities，while Jiangxi herb S1 performed poorly，providing consistent conclusions with quality evaluation. The established method provide a scientific basis for the quality control and the quality standard of C. paliurus. herb.关键词：Cyclocarya paliurus.;high performance liquid chromatography（HPLC）;fingerprint;content determination;hypoglycemic;uric acid-lowering
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发布时间：2024-07-08 -
Sensitive Detection of Telomerase Activity Based on a G-quadruplex Electrochemiluminescent Biosensor
摘要：The analysis and detection of telomerase activity is important for cancer diagnosis，prognosis，and treatment. In this study，an electrochemiluminescence（ECL） biosensor was constructed for sensitive detection of telomerase activity in cancer cells using a metal complex-targeted luminescent probe［Ir（ppy）2（pip）］PF6 for G-quadruplex（G4） DNA. Primer DNA was first assembled on the electrode surface and then co-incubated with telomerase extracted from cancer cells. The active telomerase generated telomeric repeats at the end of the primer to form the G4 structure，and then［Ir（ppy）2（pip）］PF6 bound to the extended sequence by targeting with G4. The results showed that the ECL signal of［Ir（ppy）2（pip）］PF6 showed a positive correlation with telomerase activity，and the ECL intensity of the sensor showed a good linear correlation with the concentration of cancer cells in the range of 10-5×105 cell/mL，with the limit of detection（LOD） of 3 cell/mL. The experiments also demonstrated that the sensor had good stability，applicability，anti-interference ablity，and reproducibility. Finally，the sensor was used for the determination of telomerase activity in real human serum and urine samples，and satisfactory results were also obtained.关键词：telomerase activity;G-quadruplex;metal complex;electrochemiluminescence;biosensor- 2
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发布时间：2024-07-08 - 摘要：The combination of chromatography，mass spectrometry，spectroscopy，and energy spectrum analysis techniques is used to screen，identify，and confirm the potential functional components in the“white to black”hair products. High-performance liquid chromatography was used for targeted screening of common hair dyes using. Gas chromatography-mass spectrometry（GC-MS），and ultra-high performance liquid chromatography-high-resolution mass spectrometry（UHPLC-HRMS） were used to screen for potential hair dye and melanogenic components. Under optimized screening conditions，UHPLC-HRMS identified a significant decrease in m/z 147.930 9 after 72 hours of sample placement. Based on accurate mass number，isotope distribution，and retention time，it is inferred that the component is silver ions. The content of silver element and nitrate ion was determined by inductively coupled plasma mass spectrometry and ion chromatography，and its source was analyzed based on the properties of the raw materials. At the same time，the blackening component of the product was confirmed by low vacuum thermal field emission scanning electron microscopy，and it was speculated that silver nitrate may be an important reason for the efficacy of the“white to black”product. The“white to black”hair products based on silver nitrate as the active ingredient have significant compliance and safety risks，and there is an urgent need to strengthen supervision of such products. The combination analysis model established in this article will provide technical reference for further in-depth analysis of cosmetic safety risks.关键词：“white to black”hair products;multispectral techniques;functional components;safety risk
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发布时间：2024-07-08 - 摘要：Current domestic statutory inspection methods for glucocorticoids in cosmetics included GB/T 24800.2-2009，GB/T 40145-2021 and the Safety and Technical Specification for Cosmetics（2015 edition），which covered 58 glucocorticoids in total. A method was developed to determine 48 glucocorticoids beyond statutory inspection methods in cream-based cosmetics by ultra high performance liquid chromatography-tandem mass spectrometry. After extraction and purification，samples were loaded on a Waters ACQUITY UPLC BEH C18 column（3.0 mm×150 mm，1.7 μm），where aqueous solution containing 0.2% acetic acid and methanol solution containing 0.2% acetic acid were used as mobile phases for gradient elution. After separation of target compounds，an electrospray ionization source in positive mode was used for mass analysis. All target compounds were analyzed with multiple reaction monitoring mode（MRM） and quantified by external standard method. The limits of detection（LODs，S/N≥3） and the limits of quantification（LOQs，S/N≥10） of the method for all target compounds were 0.03 μg/g and 0.1 μg/g.The correlation coefficients（r） of 48 glucocorticoids were greater than 0.995 in the range of 2.5-60 μg/L. The matrix effects（MEs） of 48 kinds of glycocorticoids in cream-based cosmetics were investigated via the addition of standard compounds to the extracted matrix solutions to make matrix standard curves. The MEs of all target compounds were within ±15%，meaning that matrix effects are not significant. The average recoveries were 80.9%-110% with relative standard deviations（RSDs，n=6） of 0.70%-9.3% under spiked levels of 1，2 and 8 times of LOQ. One positive sample was confirmed through multiple reaction monitoring（MRM）-information dependent acquisition automated（IDA）-enhance product ion（EPI） to contain 0.3 μg/g of 6β-hydroxy triamcinolone acetonide. In conclusion，pre-processing method developed in this paper is simple and feasible and measurement results for 48 glucocorticoids are accurate and reliable，which can fill the regulatory gap of illegal addition of glucocorticoids in cosmetics.关键词：ultra high performance liquid chromatography-tandem mass spectrometry;glucocorticoid;cosmetic;illegally added
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发布时间：2024-07-08 - 摘要：A method for the detection of 13 kinds of dihydropyridine calcium antagonists in antihypertensive health foods by ultra-performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） was established. Tablets and functional tea samples were extracted by ultrasonic extraction with methanol-water（4∶1） solution but methanol used by oral liquid samples. The separation was performed on a Waters ACQUITY UPLC BEH C18 column（2.1 mm × 100 mm，1.7 μm） with a gradient elution of 0.1% formic acid aqueous solution（containing 2 mmol/L ammonium formate） and acetonitrile at the flow rate of 0.4 mL/min. Electrospray ionization source was done in the positive ion mode and analytes were detected in the MRM mode to complete the detection. Thirteen analytes had a good linear relationship in their own linear ranges，and the correlation coefficients were not less than 0.998 0. The average recoveries were 85.1%-119%，the intraday relative standard deviations（RSDs） were 0.37%-5.6% and the interday RSDs were 1.6%-13%. The detection limits of each analytes in tablets，functional teas，and oral liquids were in the ranges of 0.1-2 μg/kg，0.1-5 μg/kg，and 0.1-1.7 μg/L，respectively. The 46 samples procured were tested by this method，and 2 positive samples were found，one of which detected nifedipine 178.1 μg/kg and the other detected 260.2 μg/kg of manidipine. This method is simple，high sensitivity and good precision，which is suitable for the screening and quantitative analysis of illegally added dihydropyridine calcium antagonists in health food.关键词：antihypertensive health food;dihydropyridine calcium antagonists;UPLC-MS/MS;illegal additions
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发布时间：2024-07-08 - 摘要：In this study，a highly sensitive detection method for trace evidence of condom lubricants was established using Py/GC-MS. Simulated sexual assault case samples were prepared，extracted using hexane ultrasonication，processed through membrane filtration，and evaporated under N2 flow to 50 µL. The collected extract was transferred to a pyrolysis crucible using a pipette，evaporated solvent completely，and analyzed by Py/GC-MS. Methodological investigations showed that the quantitative limit of this method was 5 µg/kg，with recoveries of 91.0% to 103% and relative standard deviations（RSDs） of 7.1% to 8.3%. The method was used to analyze PDMS standards and simulated samples made from the top 20 best-selling condoms from online sellers，assessing interference from biological fluids（blood，urine，saliva） and the persistence on different media（underwear，skin）. PDMS was detected in all silicone-based lubricated condom samples，excluding interference from blank samples. Biological fluids did not interfere with PDMS detection，and the longest attachment times in underwear and skin environments were 72 hours and 48 hours，respectively，establishing a detection time window after sexual assault incidents. This method provides an accurate and reliable way to detect trace evidence of condom lubricants.关键词：condom;lubricant;polydimethylsiloxane（PDMS）;Py/GC-MS;persistence
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发布时间：2024-07-08 - 摘要：A method was established using a rapid multiple filtrate purification column（mPFC-QuEChERS） combined with ultra-high performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） for the simultaneous determination of sixteen mycotoxins in three radix and rhizome Chinese herbal medicines. Through optimization of the liquid chromatography conditions，mass spectrometry conditions，and sample pretreatment process，the sample was extracted with a high-speed homogenizer using an 80% acetonitrile solution（containing 2% acetic acid），and single-step purified by a mPFC-QuEChERS purification column. The analytes were separated by a shim-pack Velox PFPP chromatographic column，and eluted with a gradient of 0.01% formic acid/0.2 mmol/L formic acid ammonium solution and methanol as the mobile phase，and determined in positive and negative electrospray ionization mode in multiple reaction monitoring（MRM） mode. Quantitative analysis was performed using the external standard method. Under the optimal experimental conditions，sixteen mycotoxins showed good linear relations in their mass concentrations（r>0.99），with the detection limits（LODs） ranging from 0.3 to 25 μg/kg and quantification limits（LOQs） ranging from 0.5 to 50 μg/kg. The residual levels of 16 mycotoxins were spiked at 2.5，10 and 20 times of LOQ with average recoveries ranging from 63.3% to 110% and relative standard deviations（RSDs） ranging from 0.20% to 6.7%. 60 batches of Chinese herbal medicines were detected，and the detection rate was 30%. Ochratoxin A（OTA），15-acetyldeoxynivalenol（15-ACE） and sterigmatocystin（ST） were relatively high detected. Notably，OTA was detected in 9 batches of Astragali Radix and 2 batches of Codonopsis Radix，representing the highest detection rate. The method was simple，high sensitive，and practicable，which can be used for the rapid screening and quantitative analysis of 16 mycotoxins in radix and rhizome Chinese herbal medicines.关键词：mycotoxins;mPFC-QuEChERS;UPLC-MS/MS;radix and rhizome Chinese herbal medicines
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发布时间：2024-07-08 - 摘要：In this study，an ultra performance liquid chromatography-quadrupole-time-of-flight high-resolution mass spectrometry（UPLC-Q-TOF MS） method was developed for the rapid screening and quantitative analysis of 15 prostaglandin analogues in cosmetics. The analytes in sample were dispersed in saturated sodium chloride solution（wax samples were dispersed with tetrahydrofuran），then extracted with acetonitrile. After centrifugation and filtration，the UPLC separation of 15 prostaglandin analogues was performed on Poroshell 120 EC-C18 column（150 mm×3.0 mm，2.7 μm），using 5 mmol/L ammonium formate（containing 0.1% formic acid） solution and acetonitrile as mobile phase by gradient elution. 15 prostaglandin analogues were detected by positive ion electrospray ionization（ESI） in the Targeted MS/MS mode. To construct a screening library with the software by the retention time，exact mass of primary parent ions，isotope abundance ratio and secondary sub-ion library matching were collected. The results of matching were used to rapid identification of 15 prostaglandin analogues in cosmetics. The quantification of primary parent ions was performed by external standard method. 15 prostaglandin analogues were all well separated. The linear correlation coefficients（r2） were more than 0.99. The limits of detection（LODs） ranged of 0.3-17.6 μg/g and the limits of quantitation（LOQs） ranged of 1.1-58.8 μg/g. The recoveries at three spiked levels in lotion，cream，emulsion，powder and gel matrices varied from 70.1% to 134%，with relative standard deviations not more than 7.5%. The established method is rapid，simple and accurate，which is suitable for the screening and determination of 15 prostaglandin analogues in cosmetics，providing technical support for cosmetic risk identification.关键词：ultra performance liquid chromatography-quadrupole-time-of-flight high-resolution mass spectrometry;rapid screening;cosmetics;prostaglandin analogues
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发布时间：2024-07-08 - 摘要：The method for the determination of 25 imidazole veterinary drugs and their metabolites in eggs was established by high performance liquid chromatography（HPLC）. The egg solution was extracted and concentrated by acetonitrile，purified by Oasis PRIME HLB solid phase extraction column. The samples were eluted by gradient with methanol and water as mobile phases，separated by ZORBAX SB-Aq（250 mm×4.6 mm，5 μm） column，detected by diode array detector（DAD），and quantified by external standard method. The results demonstrated that the 25 compounds showed good linear relationships in their linear ranges with the correlation coefficients（r2） greater than 0.999. And the limits of detection（LODs） and quantification（LOQs） were 0.8-5.0 μg/kg and 2.5-12.5 μg/kg，respectively. The average recoveries ranged from 78.5% to 103% and the relative standard deviations（RSDs） ranged from 1.1% to 6.5% at three concentration levels. The method has no obvious matrix effect with high accuracy and good precision，which can be used for the daily detection of 25 imidazole veterinary drugs and metabolites residues in eggs.关键词：benzimidazole;nitroimidazole;metabolite;high performance liquid chromatography;egg
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发布时间：2024-07-08
Scientific Papers
- 摘要：Surface enhanced Raman spectroscopy（SERS） was used to detect the migration of 4，4'-dichlorophenyl sulfone from plastic food contact materials. Au nanoparticles were prepared for SERS substrate and characterized，then the Raman characteristic peaks of 4，4'-dichlorophenyl sulfone were assigned by theoretical calculation. The migration behavior of 4，4'-dichlorophenyl sulfone in plastic food contact material products was carried out according to the GB 31604.1-2015 and GB 5009.156-2016. The obtained solution was passed through a 0.22 μm filter membrane，and mixed with AuNPs to perform SERS test，and the results were validated by high performance liquid chromatography（HPLC）. The intensity of the characteristic peak（748 cm-1） of 4，4'-dichlorophenyl sulfone showed a good linear relationship with the mass concentration of 4，4'-dichlorophenyl sulfone in the range of 0.05-10 mg/L，and the correlation coefficient was 0.992 8，the recoveries of SERS method were 85.2%-93.4% with the relative deviations of 4.2%-6.6%，meanwhile，these results were in good agreement with the HPLC. The proposed method was applied to the determination of 4，4'-dichlorophenyl sulfone in 5 brands of polyphenylene sulfone（PPSU） milk bottles. This method is rapid，accurate and user friendly，and provides a technical reference for the determination of 4，4'-dichlorophenyl sulfone in food contact materials and products.关键词：surface enhanced Raman spectroscopy;4，4'-dichlorophenyl sulfone;Au nanoparticles;plastic food contact material products;migration
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发布时间：2024-07-08 - 摘要：Heavy metal elements represent a significant threat to the quality safety of dairy products，making their rapid detection a focal point in food safety research. This paper introduces a novel detection method，surface enhanced scanning laser induced breakdown spectrum（SES-LIBS），for improving the detection sensitivity and throughput of heavy metals in liquid milk. The SES-LIBS utilized the principle of metal displacement reactions to enrich trace heavy metal ions in specific areas above an active metal substrate. Subsequently，LIBS scanned the specific surface area of the metal substrate to collect trace heavy metal signals in liquid milk. The SES-LIBS was capable of avoiding the plasma cancellation with the improvement of detection sensitivity for trace heavy metal ions. To overcome both interference of sample collection and matrix in SES-LIBS signals，the paper developed a reweighted characteristic spectrum driven auto-encoder siamese multitasking network（RCSD-ASMN），which accurately extracted spectral information of the interested analytes from complex and fluctuant LIBS signals. The results demonstrated that the SES-LIBS was capable of detecting multiple heavy metal elements such as Cd and Cu simultaneously，with limitation of detection of 0.11 mg/kg and 0.13 mg/kg，respectively. The linearity（R2） of the detected elements is not less than 0.97. These results revealed that the SES-LIBS methodology supressed cross-interference from different liquid milk substrates and heavy metal elements，presenting excellent detection accuracy and linearity. This would definitely provide a novel approach for high-throughput detection of heavy metals in liquid milk samples，which may well extend to other liquid systems.关键词：liquid milk;heavy metals;surface enhanced scanning laser induced breakdown spectrum;reweighted characteristic spectrum;auto-encoder siamese multitasking network
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发布时间：2024-07-08 - 摘要：The study collected 4 998 near infrared spectra of 15 types of waste textiles，which were divided into a training set and a validation set in a ratio of 7∶3，and the data were downscaled using two different downscaling methods，namely principal component analysis（PCA） and kernal principal component analysis（kernal-PCA），respectively，and the cosine similarity（cosine） kernel was selected as the best kernel function for kernal-PCA. Finally the PCA and kernal-PCA dimensionality reduction processed data are trained by k-nearest neighbour algorithm（KNN） respectively. The results show that the model accuracy of kernal-PCA +KNN（95.17%） is better than that of PCA+KNN model（92.34%） . The study shows that the kernal-PCA +KNN algorithm can achieve the improvement of the recognition accuracy of 15 types of waste textiles，and provide a strong technical support for the online near infrared automatic sorting of waste textiles.关键词：waste textiles;principal component analysis（PCA）;kernel principal component analysis（kernel-PCA）;k-nearest neighbour（KNN） algorithm;classification recognition
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发布时间：2024-07-08 - 摘要：A method was established for the detection of residues of ten aminoglycoside（AGs） drugs（apramycin，gentamycin C1，kanamycin，hygromycin B，paromomycin，amikacin，etimicin，netimicin，tobramycin and ribostamycin） in honey using high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）. Several conditions were optimized，including sample extraction and purification，chromatographic conditions and mass spectrometry parameters.The honey samples were extracted with 100 mmol/L phosphate buffer（pH 8.0） and purified with SuperMIP SPE column. The eluent was 1.0 mL acetonitrile water（20∶80，volume ratio） solution containing 5% formic acid. Furthermore，the chromatographic separation conditions and response intensities of the 10 AGs in different mobile phases were compared. The optimized HPLC conditions were as follows：Thermo Hypercarb chromatography column（150 mm×2.1 mm，5 μm）；column temperature，35 ℃；flow rate，0.35 mL/min；injection volume，10 μL；mobile phase A：5% ammonia solution；mobile phase B：acetonitrile. The samples were quantified using positive-ion multiple reaction monitoring（MRM） mode for 13 min. The AGs were quantified using an external standard with matrix calibration curves to reduce the influences of the matrix effects on the quantitative results. The calibration curves showed good linearity in the range of 20-500 μg/L，and the limits of quantification（LOQs） of ten aminoglycoside drugs in honey were 25 μg/kg. The recoveries for the analytes at three spiked levels（25，50，250 μg/kg） ranged from 73.4% to 93.2%，with relative standard deviations（RSDs）of 5.2%-11%. The method is simple，highly sensitive，and avoids the use of ion pair reagents throughout the process，effectively reducing contamination of the mass spectrometer and it is suitable for detection of aminoglycosides in honey.关键词：aminoglycosides drugs;high performance liquid chromatography-tandem mass spectrometry;MIP-SPE;honey
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发布时间：2024-07-08 - 摘要：The nitrogen-doped carbon quantum dots（N-CDs） with high fluorescence properties and fluorescence quantum yield of 89.38% were prepared by microwave one-step synthesis. A new method for the rapid and accurate determination of sulfasalazine（SSZ） was established by fluorescence quenching. The carbon quantum dots were characterized by transmission electron microscopy（TEM） and Fourier infrared spectroscopy（FT-IR）. The results showed that the average particle size of N-CDs was 2.91 nm，mainly composed of C，O and N elements，and a large number of carbonyl，hydroxyl and carboxyl groups existed on the surface of N-CDs. Under the optimal conditions，the concentration of sulfasalazine was linear in the range of 0.1-2 μmol/L and 3-200 μmol/L，and the detection limit was 0.2 μmol/L. The content of sulfasalazine in sulfasalazine enteric-coated tablets was determined by this method，and the recovery was 97.3%-102%.关键词：microwave method;nitrogen-doped carbon quantum dots;fluorescence quenching;sulfasalazine
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发布时间：2024-07-08 - 摘要：A highly stable method for the detection of glucose in serum was developed. The nanocomposite GOx/CDs@ZIF-8 was prepared by co-encapsulating glucose oxidase（GOx） and carbon dots（CDs） in a zeolitic imidazolate framework material（ZIF-8）. Under neutral conditions，this nanocomposite material can efficiently catalyze the oxidation of glucose to produce H2O2，and then free radicals（·OH） were produced via a Fenton-like reaction from the H2O2 and Co2+. The free radical can burst the fluorescence of carbon dots，based on which，a fluorescence detection method for glucose in serum was constructed. Under the optimized conditions，the detection limit of the fluorescent probe was 0.16 μmol/L，and the recoveries were 91.0%-108%. The constructed nano fluorescent probe can be used for the detection of glucose in real samples and has high stability at room temperature.关键词：nano-composite;fluorescence detection;metal-organic framework;carbon dots;glucose
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发布时间：2024-07-08
Experimental Techniques and Methods
- 摘要：Fluorescence analysis is an analytical method established based on fluorescence measurement of analyte as it provides high sensitivity，good selectivity and rapid responsibility. As a kind of fluorescent materials，environmental stimuli responsive fluorescent materials display promising prospects by virtue of their wide practical applications in chemical sensing，bio-imaging，pressure sensing，information storage，photoelectronic devices and drug delivery etc. However，most of these fluorophores suffer from a troublesome“aggregation caused quenching”（ACQ）effect，which severely inhibit their applications in practical situations. As a new type of fluorescent material developed in recent years，aggregation induced emission materials（AIE）emit extremely weak fluorescence in dispersed state but intense fluorescence as aggregates form. The emergence of AIE materials discovered as a remedy to overcome the aggregation caused quenching effect ingrained in traditional fluorophores. Besides，unique photostability，high fluorescence quantum yield and controllability also provide new ideas for fluorescence analysis. This article reviews the research progress of fluorescence analysis concerning AIE in biomedicine，chemical detection，public security accompanied with food and agriculture，and looks forward to challenges and future directions of research in this field.关键词：aggregation induced emission;biomedicine;chemical analysis;public security;food
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发布时间：2024-07-08 - 摘要：Nicotinamide adenine dinucleotide（NAD）is a key accessory molecule prevalent in all living cells and plays an important role in cellular metabolism. NAD directly controls intracellular energy metabolism，participates in DNA damage repair，regulates intracellular calcium ion concentration，and other important life processes，and plays a critical role in the metabolic reactions of cells. The study of NAD level in biological cells has been one of the research hotspots in life science research in the last 20 years. In this paper，we summarize the research progress of NAD level detection methods in biological cells from the perspectives of structural properties and synthesis pathways of NAD，introduce the principles，advantages and disadvantages，and the scope of application of various methods，and look forward to the development trend of the methods，in order to provide a good guidance for the related research.关键词：nicotinamide adenine dinucleotide（NAD） level;metabolic flow;structural characteristics;test method;review
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发布时间：2024-07-08 - 摘要：Aquaphotomics is used to explore the structure of aqueous system through water-light interaction，which takes water in the living system as the research object，uses spectral technology to detect the structural changes of water molecules in different environments，and reflects the interaction between water and other molecules in the living system or the function of water in the living system at the molecular level. In this paper，the concept and principles of aquaphotomics were introduced. including the related chemometrics algorithms and visualization models. The wide range of applications in the fields of aquaphotomics in life science, quality control of agricultural products/aquatic products/food, biochemical analysis and characterization of active substances, building materials, and traditional Chinese medicine were summarized. Finally，the current status of near infrared aquaphotomics technology and its applications was discussed，and the prospects were proposed.关键词：aquaphotomics;near infrared spectroscopy;chemometrics;visual model
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发布时间：2024-07-08
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