Adulteration of high-value oils such as olive and camellia oil poses serious challenges to market integrity and consumer safety. This study develops a comprehensive, model-free marker library for high-throughput detection of single and multivariate adulteration across nine vegetable oils (olive, camellia, sesame, rapeseed, flaxseed, soybean, peanut, industrial hemp seed, and sunflower seed oils) using untargeted metabolomics via UHPLC-Q-TOF-MS. We identified 34 characteristic markers, including 9 confirmed by reference standards, such as hydroxytyrosol in olive oil, camelliasaponins in camellia oil, and sesamin in sesame oil, which are uniquely present in specific oils and absent in others. The method enables reliable qualitative screening of adulteration at levels as low as 5% without dependence on chemometric models. Validation using binary and multicomponent blends confirmed its robustness and specificity. In commercial sample analysis, adulteration was detected in 16.0% of olive oils (4/25) and 12.7% of camellia oils (7/55), with results consistent with regulatory findings. This work establishes the first integrated marker library for simultaneous screening of nine vegetable oils, offering a standardized, high-throughput tool for large-scale market surveillance that bridges the gap between discovery-based omics and routine regulatory practice.
Type 1 diabetes mellitus (T1DM) is an autoimmune disease, and its symptoms are influenced by oxidative stress and inflammation. This study characterized the main active component of Typha latifolia, Typha latifolia polysaccharide (TLP), and explored its mechanism for improving type 1 diabetes at the mRNA level. We have characterized the preliminary structural characterization of TLP through Fourier transform infrared spectroscopy, monosaccharide composition analysis, methylation analysis, and nuclear magnetic resonance. Through in vitro and in vivo experiments, it was confirmed that Typha latifolia polysaccharide (TLP) improves T1DM through multi-target synergistic effects, including increasing serum insulin levels, improving glucose tolerance, and regulating the expression of liver GK/G6Pase to improve glucose metabolism disorders. Meanwhile, RT-qPCR results indicate that at the mRNA level, it demonstrates the ability to inhibit the TLR4/NF-κB pathway to alleviate inflammation and activate the Nrf2/HO-1 pathway to mitigate oxidative stress. In addition, TLP can also reshape the intestinal flora, increase the abundance of beneficial bacteria such as Akkermansia, and promote the production of short-chain fatty acids, thereby comprehensively regulating blood glucose, inflammation and metabolic functions, and ultimately achieving the effect of improving T1DM.
The purpose of this study is to explore chitosan with Stachys floridana Shuttlew. ex Benth (SFSB) extract as an additive to prepare an active film. The effects of the SFSB extract on the physical, antioxidant, and bacteriostatic properties of chitosan biodegradable films were studied. The results showed that the addition of SFSB extract significantly improved the antioxidant and antibacterial properties of the film, and its biodegradation rate increased rapidly. Compared to the control film, the water solubility was lower at 19.40%, the expansion degree was higher at 288.90%, the water vapor permeability (WVP) was 0.364 g·mm/(m²·d·kPa), the surface hydrophobicity increased, and the mechanical strength was also improved. The contact angle increased to 89.3°. In addition, as the amount of SFSB increased, the thermal stability of chitosan-Stachys floridana Shuttlew. ex Benth (CS-SFSB) films also increased significantly, and their ultraviolet (UV) blocking ability was gradually enhanced. The results indicate that CS-SFSB has potential as a food packaging material.
Lactuca indica L. is both edible and medicinal, and has various effects such as antioxidant and anticardiovascular diseases. Lactuca indica L. polysaccharide (LIP) is the active constituent of Lactuca indica L. The goal of this study was to provide a preliminary analysis of the structural properties of LIP and to investigate its therapeutic efficacy and possible mechanisms in STZ-induced T1DM. This study isolated a homogeneous polysaccharide, designated LIP, from the crude polysaccharide of Lactuca indica L. This polysaccharide is an acidic polysaccharide consisting of eight monosaccharides. LIP has significant therapeutic effects on T1DM mice, can regulate abnormal glucose metabolism, inhibit excessive inflammation, and alleviate pancreatic and hepatic damage. Furthermore, LIP modulated hepatic insulin signaling and inflammatory pathways, as well as restored the balance of the intestinal microbiota, particularly with regard to the increase in SCFAs-producing bacteria. There is a significant correlation among them. In conclusion, LIP may be a candidate agent to treat diabetes.
Health wines are alcoholic beverages produced by infusing traditional liquors or rice wines with natural, medicinal, and food-safe ingredients. However, to accelerate efficacy, some manufacturers illegally adulterate health wines with phosphodiesterase type 5 (PDE-5) inhibitors, which may cause severe adverse effects. This study developed a method based on ultra-high-performance liquid chromatography–time-of-flight mass spectrometry (UPLC–TOF/MS) for the rapid screening and identification of 68 PDE-5 inhibitors illegally added to health wines. After optimizing the sample preparation procedure, chromatographic conditions, mass spectrometric parameters, and primary and secondary mass spectra of the 68 PDE-5 inhibitors were acquired as reference standards. Retention times and mass spectral data were imported into the Personal Compound Database and Library, establishing a high-resolution screening database with matched drug names, molecular formulas, and accurate molecular weights. A quantitative method was validated using 11 commonly adulterated compounds, including sildenafil. The response was highly linear (r ≥ 0.9988; 0.8–400 μg/L) with low detection limits (0.2–1.0 μg/L). The average spiked recoveries were 71.2–104.1%, with relative standard deviations of ≤10.1%. Among 59 commercial health wine samples, three batches tested positive for PDE-5 inhibitors (detection rate: 5.1%). The proposed method can assist market surveillance even when reference standards are unavailable for all compounds.
PURPOSE:In this experiment, we investigated the effect of Pyrus pashia Buch on the relevant inflammatory disease indexes, intestinal microbiota, and short-chain fatty acids in mice with dextran sodium sulfate (DSS)-induced ulcerative colitis. METHODS:The anti-inflammatory effect of PPBP was assessed by measuring inflammatory markers (ELISA), colonic pathological changes (H&E), qPCR of relevant gene expression, 16S rRNA sequencing of intestinal contents, and short-chain fatty acids (SCFAs). RESULTS:Pyrus pashia Buch polysaccharide (PPBP) alleviated the main symptoms of UC (Weight down, reduced diet, increased disease activity index) and ameliorated pathological damage to colonic tissues by reducing the release of cytokines TNF-α, IL-6, IL-1β, and iNOS. Furthermore, PPBP enhanced the expression of tight junction proteins (ZO-1, Occludin, and Claudin-1) and elevated intestinal mucin MUC2 and MUC3 levels. qPCR analysis showed that PPBP activated MAPK/NF-κB and verified that it regulated the MAPK signaling pathway through the SCFA-ERK-MSK pathway and downregulated the phosphorylation levels of p38 and p65. Using the 16S rRNA method to analyze the level of microbial changes in the mouse gut, it was shown that Pyrus pashia Buch polysaccharide (PPBP) restored the intestinal microbial diversity and species richness in the UC model, and gas chromatography-mass spectrometry analysis demonstrated that Pyrus pashia Buch polysaccharide (PPBP) was able to increase beneficial short chain fatty acids. CONCLUSION:PPBP is a resourceful edible herb. By studying the mechanism of action of P38/IκBα/P65 in MAPK/NF-κB and SCFA with ERK/MSK in MAPK, we have demonstrated that PPBP can attenuate inflammatory responses to repair intestinal mucosal damage, balance abnormalities in the intestinal microbiota, and improve the function of the damaged intestinal barrier. It provides preliminary experiments for developing PPBP as an IκBα stabilizer and P65 inhibitor.
Abstract This project presents a quantitative detection method to identify raccoon‐derived ingredient adulteration in sausage products. The specific copy gene of the raccoon was selected as the target gene. According to the specificity of its primer and probe, the quantitative detection method of raccoon microdrops by droplet digital PCR was established. In addition, the accuracy of the proposed method was verified by artificially mixed samples, and the applicability of this method was tested based on the commercially available products. The experimental results indicate that the raccoon mass (M) and raccoon‐extracted DNA concentration have a good linear relationship when the sample content is 5–100 mg, and there is also a significant linear relationship between DNA content and DNA copy number (C) with R2 = .9982. Therefore, using DNA concentration as the median signal, the conversion equation between raw raccoon mass (M) and DNA copy number (C) could be obtained as follows: M = (C + 177.403)/16.954. The detection of artificially mixed samples and commercial samples shows that the method is accurate and suitable for quantitative adulteration detection of various sausage products in the market.
This paper aims to establish a rapid and accurate method to identify the adulteration of camellia oil and olive oil based on characteristic substances. The results showed that the sesamin and sesamolin can be selected as the characteristic substances of sesame oil, and oryzanol is identified as the characteristic substances of rice oil. A high-performance liquid chromatography (HPLC) method with UV determination was developed to detect the characteristic substances, which can identify whether sesame oil and rice oil are mixed in camellia oil or olive oil. The pretreatment and chromatographic conditions were optimized. The linear equation, LOD, LOQ, recovery and precision were studied. The LODs of sesamin, sesamolin and oryzanol were determined to be 25mg/kg, 50mg/kg and 50mg/kg, respectively. Similarly, the LOQs of sesamin, sesamolin and oryzanol were 50mg/kg, 100mg/kg and 100mg/kg respectively. The simulated adulterated oils with different proportion were analyzed to validate the effectiveness of method. The adulteration limit of sesame oil is 2%, and that of rice oil is 5%. The method has the advantages of simple operation, good specificity and high accuracy. It can provide technical support for oil quality control and adulteration identification.
This paper reported a novel approach to quantification of adulterated fox-derived components in meat products by drop digital polymerase chain reaction (ddPCR). By using the F2 gene as the target gene of fox, a single primer was designed to identify the adulteration that had been added either inadvertently or deliberately during the process. In this paper, the fox meat was used as the experimental materials and a relationship was established between fox mass and copy number by extracting DNA and using DNA concentration as an intermediary. The results that across the dynamic range, the relationships between meat mass and DNA concentration were nearly linear (R2 = 0.9986), as was the relationship between DNA concentration and DNA copy number (R2 = 0.9992). Based on the DNA concentration, the following formulas were developed about the relationship between fox meat mass (Mfox) and DNA copy number (C): Mfox = 0.05C + 2.7.
建立了防晒化妆品中15种香豆素与10种二苯甲酮类化合物的QuEChERS/超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法.防晒霜、粉底、隔离、喷雾等不同类型的化妆品样品采用乙腈提取,50 mg C18与150 mg无水MgSO4吸附剂净化.采用Zorbax SB-C18(RRHD)色谱柱(2.1 mm×150 mm,1.8 μm)分离,0.1%甲酸水溶液(含5 mmol/L乙酸铵)和乙腈为流动相梯度洗脱,电喷雾离子源正离子模式、多反应监测扫描模式进行测定,外标法定量,粉底和喷雾样品以基质匹配标准溶液外标法定量.结果显示,25种待测组分在各自质量浓度范围内线性关系良好,相关系数(r)均不低于0.995.对于防晒霜和隔离类样品,方法检出限(LOD)为0.005~0.450 μg/g,定量下限(LOQ)为0.010~0.750 μg/g;对于粉底与喷雾类样品,方法检出限为0.005~0.500 μg/g,定量下限为0.010~1.000 μg/g.25种待测组分的平均回收率为80.8%~113%,相对标准偏差为0.20%~6.8%.样品溶液中25种待测组分在48 h内稳定.该方法前处理简单、灵敏、准确,适用于化妆品中香豆素与二苯甲酮类化合物的同时检测.
Dental calculus is a potential material that can be used for assessing chronic exposure to trace heavy metals in oral cavity as it is a long-term reservoir. The aim of this study was to investigate the correlation between dental calculus copper levels and risk of oral submucous fibrosis (OSF) due to chewing dried areca-nut quids in Mainland China. This study included 34 OSF (grade 1) sufferers with dried areca-nut quids chewing as the patient group and 23 healthy individuals without areca-nut chewing as the control group. The dental calculus sample was obtained from all 57 participants and evaluated by inductively coupled plasma mass spectrometry (ICP-MS) for dental calculus level of copper. This work revealed that the mean copper level of dental calculus was significantly higher in OSF (grade 1) sufferers with areca-nut chewing than those in healthy individuals without areca-nut chewing (p < 0.001). This work provided an evidence to support that there may be a positive correlation between elevated levels of copper in dental calculus caused by chewing dried areca-nut quids and an increased risk of developing OSF in Mainland China.
Patulin (PAT) is a mycotoxin, with several acute, chronic, and cellular level toxic effects, produced by various fungi. A limit for PAT in food of has been set by authorities to guarantee food safety. Research on PAT in tea has been very limited although tea is the second largest beverage in the world. In this paper, HPLC−DAD and GC−MS methods for analysis of PAT in different tea products, such as non-fermented (green tea), partially fermented (oolong tea, white tea, yellow tea), completely fermented (black tea), and post-fermented (dark tea and Pu-erh tea) teas were developed. The methods showed good selectivity with regard to tea pigments and 5-hydroxymethylfurfural (5-HMF) and a recovery of 90–102% for PAT at a 10–100 ppb spiking level. Limit of detection (LOD) and limit of quantification (LOQ) in tea were 1.5 ng/g and 5.0 ng/g for HPLC−UV, and 0.25 ng/g and 0.83 ng/g for GC−MS. HPLC was simpler and more robust, while GC−MS showed higher sensitivity and selectivity. GC−MS was used to validate the HPLC−UV method and prove its accuracy. The PAT content of 219 Chinese tea samples was investigated. Most tea samples contained less than 10 ng/g, ten more than 10 ng/g and two more than 50 ng/g. The results imply that tea products in China are safe with regard to their PAT content. Even an extreme daily consumption of 25 g of the tea with the highest PAT content (124 ng/g), translates to an intake of only 3 μg/person/day, which is still an order of magnitude below the maximum allowed daily intake of 30 µg for an adult.
建立了测定酵米面和银耳及其制品中的毒黄素和热诚菌素的高效液相色谱法.样品经提取后,以C18色谱柱分离目标化合物,保留时间和光谱图定性,外标法定量.对建立的方法与现有的方法进行了对比,同时比较了两种目标物在不同条件下的稳定性.结果表明:两种目标物在0.20~20.00 mg/L浓度范围内呈良好线性,R2>0.999,检出限分别均为0.15 mg/kg(酵米面)和0.30 mg/kg(银耳及其制品),方法回收率为79.77%~104.36%,相对标准偏差(RSD)为0.96%~8.91%(n=6).毒黄素和热诚菌素在碱性条件下含量均迅速降解至40%以下,毒黄素在酸性条件下会在5个月内降解至26%以下,而热诚菌素在酸性条件下以及两者在甲醇溶液中5个月内稳定性较好,吸光值RSD均小于3.18%.该方法较现有的方法简便快捷、干扰小、准确度高,可应用于酵米面和银耳及其制品中的毒黄素和热诚菌素的检测.稳定性试验可为后期的解毒或避毒提供有力的参考.
通过优化样品前处理方法,建立了高效液相色谱法测定植物油中的毒黄素、路霉素和热诚菌素的含量.样品采用甲醇液液萃取、氮吹浓缩,经高效液相色谱仪分析检测,外标法定量.采用Ultimate AQ-C 18(4.6 mm×250 cm,5μm)色谱柱分离,流速为1.0 mL/min,流动相为0.1%甲酸-甲醇(90:10),检测波长为240 nm.在优化条件下,3种目标化合物在0~40.0 μg/mL线性范围内线性良好;毒黄素、路霉素和热诚菌素的方法检出限(S/N≥3)均为0.8 mg/kg,方法定量限(S/N≥10)均为3.2 mg/kg;在3.2~32 mg/kg的添加范围内,毒黄素的回收率为98.93%~109.44%,方法精密度(RSD,n=6)小于6.81%;路霉素的回收率为102.85%~109.77%,方法精密度(RSD,n=6)小于4.26%;热诚菌素的回收率为95.26%~101.54%,方法精密度(RSD,n=6)小于4.30%,所测11种食用植物油样品中3种目标化合物均未检出.本方法简便、准确、精密度和回收率好,可用于食用植物油中毒黄素、路霉素和热诚菌素的检测.
文章采用高效液相色谱法(HPLC)对白酒和植物油中的苯二甲酸、间苯二甲酸和邻苯二甲酸进行了测定.白酒中残留物经加热去醇、植物油中残留物经甲醇提取,离心后,在YMCC30色谱柱(250 mm×4.6 mm,5 μm)上进行苯二甲酸类的分离,供HPLC测定,外标法定量.结果表明,在流动相为75 mmol/L磷酸二氢钾-甲醇(80∶20,v/v),流速0.6 mL/min,检测波长240 nm条件下,对苯二甲酸、间苯二甲酸和邻苯二甲酸在0.4~20 μg/mL质量浓度范围内线性关系良好,相关系数在0.9996~0.9999之间,白酒的回收率在87.53%~102.96%之间,植物油的回收率在88.13%~109.12%之间,RSD小于3.0%,所测10个白酒样品以及10个植物油样品中未检出对苯二甲酸、间苯二甲酸和邻苯二甲酸.该方法操作简便、准确度高、回收率高,可用于白酒和植物油中对苯二甲酸、间苯二甲酸和邻苯二甲酸的测定.
目的:采用超高效液相色谱-飞行时间质谱联用技术(UPLC-Q-TOF-MS/MS)对丹膝颗粒中的化学成分进行定性分析.方法:采用Atlantis?T3色谱柱(2.1 mm×250 mm,5μm),以乙腈-0.1%甲酸溶液为流动相进行梯度洗脱,流速为0.4 mL/min,柱温35℃,进样量2μL.质谱采用电喷雾(ESI)离子源,正、负离子模式监测,通过保留时间、相对分子质量、质谱碎片等信息,结合对照品碎片裂解规律及文献数据对检测到的化学成分进行定性分析.结果:由一级MS、二级MS/MS高分辨质谱数据共鉴定和推测出102个化合物.结论:首次利用UPLC-Q-TOF MS/MS技术对丹膝颗粒的主要成分进行定性分析,为其质量控制、药效物质基础、药理作用机制研究提供了参考.
There are still large research gaps in the testing standards for non-edible meat-derived components at present. Here we report a novel approach to quantification of adulterated fox-derived components in meat products by drop digital polymerase chain reaction(ddPCR). It was better to identify the adulteration that has been added either inadvertently or deliberately during the process by designing single primers on housekeeping genes. In this paper, the fox meat was used as the experimental materials and the relationship between sample quality and copy number was established by extracting DNA and using DNA concentration as an intermediary. The results of ddPCR showed that both the relationships between meat weight and DNA concentration and between DNA concentration and DNA copy number (C) were nearly linear within the dynamic range. The DNA concentration was utilized as an intermediate value to establish the formulae about the relationship between the original meat weight and DNA copy number: Mfox=0.05C+2.7. The method’s feasibility was validated using artificial adulteration of different proportions The establishment of this method provides technical support for relevant regulatory authorities to monitor the adulteration of fox meat.
A method using ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was developed for the determination of toxoflavin and fervenulin in 6 types of food.The limits of detection (LODs, S/N ≥ 3) of toxoflavin and fervenulin reached 12 µg/kg and 24 µg/kg, respectively.The recoveries ranged from 70.1 % to 108.7 %.Intra-day RSDs (n = 5) and inter-day RSDs (n = 3) ranged from 0.9 % to 9.5 %.The method was successfully applied to analyse 36 samples, and one Tremella fuciformis Berk. sample was found with 7.5 mg/kg toxoflavin and 3.2 mg/kg fervenulin. Toxoflavin and fervenulin were acidic compounds and easily degraded in 0.1 % ammonia solution (v/v),degradation products were identified by ultra-high performance liquid chromatography-tandem quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF/MS).
A solid phase extraction-liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) method was developed for simultaneous determination of fructose, glucose and sucrose in tea. Tea samples were ultrasonically extracted with ultrapure water and cleaned up by Oasis PRIME HLB SPE cartridge. The separation of the analytes was performed on XBridge BEH Amide column (2.1 x 150 mm, 5 mu m) with isocratic elution. Detection of the target compounds were carried out under the multiple reaction monitoring (MRM) mode with negative electrospray ionization (ESI-). The qualitative screening was achieved with retention time and qualitative ion, then confirmation analysis with peak area and quantitative ion. The limits of detection (LODs, S/N >= 3) of fructose, glucose and sucrose were 0.02 mg/L, 0.03 mg/L and 0.08 mg/L, respectively. The average recoveries varied from 92.1 %-108.5 % for three levels. Linearity was obtained with the correlation coefficients greater than 0.992 for three target compounds. The established method was rapid, simple and accurate which was suitable for batch determination of fructose, glucose and sucrose in tea. A total of 213 tea samples from 7 countries were analysed and the results statistically analyzed using MATLAB software. Moreover, source and adulteration analysis of sucrose in tea was carried out. Sucrose in tea is mainly derived from photosynthesis during growth, hydrolysis of polysaccharides during the processing and artificial adulteration, once the sucrose content in tea exceeds 24.3 g/kg, it may involve artificial adulteration.