Liquid crystal monomers (LCMs) are emerging environmental contaminants with bioaccumulation potential and health risks. Chinese herbal medicines, susceptible to LCM uptake during cultivation or processing, represent a potential human exposure route. However, reliable methods for analyzing LCMs in these complex matrices are lacking. Herein, a modified QuEChERS method coupled with gas chromatography-tandem mass spectrometry (GC-MS) was developed for the determination of 10 LCMs in herbal medicines. Samples were extracted with dichloromethane and cleaned up using mixed sorbents (N-propyl ethylenediamine and octadecylsilane). The method showed excellent linearity (2.0-200.0 mu g/L, r(2) > 0.999), with limits of detection and quantification of 0.5-2.0 mu g/kg and 1.0-5.0 mu g/kg, respectively. Mean recoveries across three spike levels in different matrices ranged from 75.0% to 112.9%, with relative standard deviations of 2.0-8.5% (n = 6). In the analysis of 26 real herbal medicines samples, LCMs were detected in mulberry leaf and Salvia miltiorrhiza, indicating a detection frequency of 7.7% and potential contamination in herbal medicines. This reliable and practical method is suitable for routine monitoring of LCM residues in various herbal products.
A headspace solid-phase microextraction (HS-SPME) coupled with comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC×GC-TOF MS) was established to scientifically evaluate the composition and potential safety risks of volatile organic compounds (VOCs) in polylactic acid (PLA) straws. The effects of different SPME fiber, equilibration temperature, equilibration time, and extraction time on extraction efficiency were systematically investigated. The results showed that DVB/C-WR/PDMS was selected as the optimal extraction fiber. After equilibration at 100℃ for 30 min and adsorption for 20 min, and a total of 193 VOCs were identified from the 18 PLA straw samples. According to their structures, these VOCs can be classified into 10 categories: alkanes, alkenes, esters, benzene series, alcohols, aldehydes, ketones, phenols, naphthalenes, and others. Among these, 43 substances were detected at high frequency. Following toxicity classification, they comprised 12 substances of Class III toxicity and 7 substances of Class IV toxicity, with the remainder falling under Class I or Class II. The HS-SPME/GC×GC-TOF MS method established in this study can be effectively used for comprehensive screening and qualitative analysis of VOCs in PLA straws, providing a scientific basis for the safety assessment of volatile components in PLA straws.
A head-space solid phase micro-extraction combined with comprehensive two-dimensional gas chromatographtandem quadrupole-time-of-flight mass spectrometry (HS-SPME/GC & times; GC-QTOF MS) was established to assess the composition and potential safety risks of volatile organic compounds (VOCs) in polylactic acid (PLA) straws. The effects of different SPME fibers, equilibration temperature, equilibration time, and adsorption time on extraction efficiency were systematically optimized. The results indicated that DVB/C-WR/PDMS was the optimal extraction fiber. Under the optimal conditions (equilibration at 1000 degrees C for 30 min and adsorption for 20 min using the DVB/C-WR/PDMS fiber), a total of 193 VOCs were identified from the 18 PLA straw samples. Based on their structures, these VOCs can be classified into 10 categories: alkanes, alkenes, esters, benzene derivatives, alcohols, aldehydes, ketones, phenols, naphthalenes, and others. Notably, 43 compounds were detected at high frequency. Following toxicity classification, they comprised 12 compounds of Class III toxicity and 6 compounds of Class IV toxicity, with the remainder classified as Class I or Class II. Consequently, the HSSPME/GC & times; GC-QTOF MS method developed in this study proves effective for the comprehensive screening and qualitative analysis of VOCs in PLA straws, offering a scientific basis for their safety assessment.
Musk macrolides area kind of rare flavors structurally featuring 14-16 membered rings in the flavour and fragrance industry. While various chemical synthesis routes for musk macrolides exist, there is a growing interest in biocatalytic approaches. In this study, anew biocatalytic approach is proposed for the synthesis of musk macrolides from fatty acids using unspecific peroxygenases (UPOs) in combination with lipase. Specifically, the UPO from Marasmius rotula (MroUPO) was utilized as an oxidation catalyst together with the choline oxidase from Arthrobacter nicotinate (AnChOx) for the in situ generation of H2O2. The enzymatic cascade process involved the hydroxylation of fatty acids using MroUPO as a catalyst to prepare terminal hydroxylated fatty acids. Under the optimized conditions, 14-hydroxy tetradecanoic acid, 15-hydroxy pentadecanoic acid and 16-hydroxy hexadecanoic acid were obtained at concentrations of 11.1, 18.2 and 17.1 mg/L in a 50-mL reaction system, respectively. These hydroxylated fatty acids were then separated and esterified by lipase Novozymes 435 to produce the desired macrolides. Various omega-hydroxy fatty acids were successfully converted into macrolides, with the concentrations of cyclotetradecanolide, cyclopentadecanolide and cyclohexadecanolide reaching 11, 29 and 23 mg/L, respectively, in a 10-mL reaction system. This new biocatalytic approach represents a promising method for synthesizing valuable natural flavour compounds. (c) 2026 The authors. Publishing services by Elsevier B.V. on behalf of KeAi Communications Co., Ltd. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
The magnetic fluorinated graphene (Fe3O4/FG) was prepared by one-step solvothermal method and applied as adsorbent material for enrichment and purification of 12 kinds of fluoroquinolone drugs (FQs) in water and milk samples, then the FQs were detected by high-performance liquid chromatography combined with quadrupole/orbitrap high-resolution mass spectrometry (HPLC-Q/Orbitrap HRMS). The morphology, crystal structure, magnetic strength, and specific surface area of Fe3O4/FG were systematically characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), vibrating sample magnetometer (VSM), and specific surface area analyzer (BET). The single factor optimization method was used to optimize the magnetic solid-phase extraction (MSPE) parameters such as adsorbent dosage, extraction time, ion strength, sample pH, type and volume of elution. Under optimal conditions, due to the synergistic effect of the surface pi-electrons system and fluorine (F) atoms on the surface of FG, Fe(3)O(4/)FG exhibited excellent adsorption performance by generating various forces such as err-err-conjugation, F-F interactions, and hydrogen bonding with FQs. The methodological validation results showed that the 12 kinds of FQs had good linear relationships, with correlation coefficient (R-2) >= 0.999. The method limits of detection (MLOD) of 12 kinds of FQs in water and milk samples were 3-6 ng/L and 75-150 ng/L, respectively, and the method limits of quantification (MLOQ) were 10-20 ng/L and 250-500 ng/L, respectively. The established method was applied to determination of 12 kinds of FQs in water and milk samples, with spiked recoveries of 79.3%-108.4% and relative standard deviations (RSDs, n=3) of 1.5%-8.6% in water samples, and spiked recoveries of 75.6%-105.4% and RSDs (n=3) of 2.3%-9.5% in milk samples.
Inhibitory effects of litchi shell polyphenols (LC) and their characteristic catechins on 2-amino-1-methyl-6-phenylimidazole [4,5-b] pyridine (PhIP) formation were investigated in chemical model and roast pork patty. Eight catechins-adducts were identified by UPLC-Q-TOF-MS and their toxicity were evaluated by Discovery Studio. Results showed inhibition rates of LC on bound-PhIP could reach 10.95 % and 100 % respectively in both chemical model and roast pork patty, and inhibition rates on free-PhIP could reach 76.47 % in roast pork patty. However, LC had no inhibiting effect on free-PhIP, and even promoted it in chemical model. UPLC-Q-TOF-MS indicated that Epicatechin (EC), Epigallocatechin (EGC) and Epigallocatechingallate (EGCG) eliminate PhIP by capturing phenylacetaldehyde to form adducts. LD50 of the formed adducts were lower than the chronic rat oral loael value, indicating that EC, EGC and EGCG would not form more toxic adduct during PhIP reduction. This study provides a new perspective for the application of LC in inhibiting PhIP and a reference for improving the theoretical system of dietary polyphenols in inhibiting heterocyclic aromatic amines.
Hydrocolloids are another potential exogenous additive and shows efficient effect in minimizing the formation of toxic by-products during high-temperature processing attribute to their unique structure and high solubility. Therefore, this review provided for the first time comprehensive summary and proposed new insights into the inhibitory effect and mechanism of hydrocolloids on HAAs formation in meat products. Effects of the combined use of hydrocolloids and polyphenols on the HAAs formation inhibitory effects were discussed and highlighted as well. Hydrocolloids, used alone or with polyphenols, can effectively inhibit HAAs formation. Among some common hydrocolloids, carrageenan and chitosan have significant inhibition effect on HAAs formation. Their water retention properties, free radical scavenging ability, and inhibition of Maillard reaction were elucidated as the in-depth mechanism for inhibiting the HAAs formation. This review can provide theoretical reference for hydrocolloids effectively controlling HAAs formation in thermal-processed food, and reducing their harm to human health.
A schematic of the established method for the extraction and detection of l - and d -carvone in herbaceous plants.
Nitrosamines have been widely detected in various meat, poultry and fish products. This review provided an in-depth analysis on the nitrosation mechanisms of nitrosamines in meat, poultry and fish products, revealing the specificity of nitrosamines generation across different food types. The mechanisms by which nitrosamines form harmful adducts within human cells were also discussed. Nitrosamines levels in various meat, poultry and fish products and effective strategies for their control were also summarized. Reducing precursor levels, blocking nitrosamines formation pathways, and promoting nitrosamines degradation are the main control strategies. Notably, developing starter cultures to replace traditional nitrites as additives has become a focal point of research. In addition, the significant potential of lactic acid bacteria in reducing nitrosamines levels in meat, poultry and fish products has been highlighted. This review gave a comprehensive and scientific reference for understanding the formation mechanism and control of nitrosamines in meat, poultry and fish products.
The consumption of tangerine peel (Citri reticulatae pericarpium, CRP) has been steadily increasing worldwide due to its proven health benefits and sensory characteristics. However, the price of CRP varies widely based on its origin, variety, and aging time, which has led many manufacturers to offer inferior products by exploiting the sensory similarity of CRP, seriously undermining consumers' interests. Therefore, it is essential to identify the authenticity of the CRP. In this study, the research progress on the authenticity of CRP from different origins, years and varieties over the past 10 years and the application and prospects of the main technologies and techniques were reviewed. The advantages and disadvantages of the commonly used methods were also summarized and compared. Mass spectrometry-based and spectroscopy-based techniques are the most commonly used methods for analyzing CRP authenticity. However, designing fast, non-destructive and green methods for identifying CRP authenticity would be the future trend.
Emerging biodegradable food contact materials (FCMs) are omnipresent in food handling and processing. However, similar to conventional FCMs, small molecules can migrate into the food matrix during contact. Extensive evaluation of the migration of chemicals, added intentionally and non-intentionally, from FCMs into food is a crucial step in the safety assessment of such materials. In this study, non-targeted screening was first performed to analyze migrants from poly(butylene adipate-co-terephthalate)/modified starch (PBAT/MFS) FCM using gas chromatography–mass spectrometry and ultra-performance liquid chromatography-Q Exactive Plus Hybrid Quadrupole-Orbitrap mass spectrometer. Sixteen volatile migrants were identified, and 134 non-volatile compounds were screened for dissolution precipitates and food simulants using a self-built and commercially-available databases. The risk ranking for migrants revealed that 13 small molecules had high scores and were assigned as Risk I substances of great concern. Among them, pesticide residues and mycotoxins non-intentionally introduced from MFS blending are of great concern.
目的 基于超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)建立乳制品中乳铁蛋白、乳桥蛋白、奶牛 A1 β-酪蛋白和 A2 β-酪蛋白、水牛 A2 β-酪蛋白的检测方法,开展市售乳制品中功能性蛋白质检测和乳制品真实性鉴评分析.方法 乳蛋白经酶解后,应用超高效液相色谱-四极杆-静电场轨道阱高分辨质谱法(ultra performance liquid chromatography-triple quadrupole-Orbitrap high resolution mass spectrometry,UPLC-Q/Orbitrap HRMS)和UPLC-MS/MS筛选获得可用于定性定量分析的特征肽段,基于 UPLC-MS/MS建立同时检测 LF、LPN、奶牛A1 β-CN、奶牛A2 β-CN和水牛A2 β-CN的方法并应用于乳制品检测.结果 5 种待测蛋白在相应的浓度范围内线性关系良好(r2>0.99),加标回收率在 82.1%~105.5%之间,相对标准偏差均小于 5%,78 份乳制品的检测结果表明同类样品LF含量差异较大,不同类液体乳中LPN均值差异不大.结论 本方法性能良好,适用于乳制品中乳桥蛋白等功能性蛋白的同时检测,也可以实现乳制品中乳蛋白物种来源的鉴别.
建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定动物源食品中氟啶虫胺腈和氟吡呋喃酮残留量的方法.样品中的氟啶虫胺腈和氟吡呋喃酮经乙腈超声提取和分散固相萃取净化,净化后的样液经滤膜过滤后采用UPLC-MS/MS法测定.以乙腈和5 mmol/L乙酸铵-0.1%甲酸水溶液为流动相,采用ACQUITY UPLC? HSS T3色谱柱(2.1 mm×100 mm,1.8 μm)分离,电喷雾离子化、正离子扫描方式和多反应监测模式检测,外标法定量.结果表明,氟啶虫胺腈和氟吡呋喃酮在0.25~20.0 μg/L范围内线性关系良好,相关系数(r2)分别为0.9993和0.9991,方法检出限和定量下限分别为1.0 μg/kg和5.0 μg/kg.实际样品的平均加标回收率为90.1%~113%,相对标准偏差(RSD)为2.5%~7.8%.该方法快速简便、准确度和灵敏度高、重现性好,可满足动物源食品中氟啶虫胺腈和氟吡呋喃酮残留的检测要求.
以市售红烧乳鸽为研究对象,建立超高效液相色谱-四极轨道高分辨质谱(UHPLC-Q-Orbitrap HRMS)联用法,并对红烧乳鸽样品中不同部位11种极性杂环胺含量进行检测.结果表明:建立的方法线性关系良好、灵敏度较高,11种杂环胺的质量准确度均<3×10-6,决定系数R2≥0.9972,方法的检出限为0.03~0.60μg/kg,定量限为0.10~2.00μg/kg;该方法具有稳定的回收率和一定的精确性,11种杂环胺的回收率为83.40%~114.80%,精密度为1.40%~7.20%,结果良好;红烧乳鸽中主要检出MeIQx(0.10~0.46μg/kg)、PhIP(0.10~0.53μg/kg)和DMIP(0.10~0.25μg/kg)3种杂环胺,乳鸽部位中HAAs总含量由多到少依次为鸽跟>鸽胸>鸽翅>鸽腿.
PhIP (2-amino-1-methyl-6-phenylimidazole [4, 5-b] pyridine) is a carcinogenic heterocyclic aromatic amine often generated in thermal processing of food. Methods for PhIP and its precursors and possible intermediates determination in chemical model system and roast pork were established based on HPLC-Q-Orbitrap-HRMS and GC-MS. Results showed that the linearity of 8 targets was good in a certain concentration range (R2 & GE; 0.992). LODs and LOQs were in the range of 0.3-15 & mu;g/kg and 1-50 & mu;g/kg, respectively. Under the model system, the recoveries of 8 target compounds ranged from 86.3% to 119.2%, with relative standard deviations (RSDs) of 0.5-6.9%. The established method was applied to 8 targets determination in roast pork, with recoveries ranging from 87.1% to 107.3% and RSDs in the range of 1.2-7.8%. The developed methods are accurate and fast, which are suitable for PhIP and its precursors and possible intermediates analysis in chemical model system and actual meat products.
Exposure to heavy metals exerts toxic effects on female reproduction and embryo development. This study examined the exposure of patients with unexplained recurrent miscarriage (uRM) to multiple metals and the correlations among exposures to different metals. A total of 275 participants were enrolled, including 43 healthy women without previous miscarriage (the control group) and 232 uRM women (the case group); among these uRM women, 159 had two miscarriages (2M), 42 had three miscarriages (3M) and 31 had four or more miscarriages (≥4M). A total of 22 elements were measured in serum samples via inductively coupled plasma–mass spectrometry. The levels of calcium (104.37 mg/L vs. 92.65/93.02/92.61/92.47 mg/L) and selenium (131.85 µg/L vs. 117.80/118.04/115.88/124.35 µg/L) were higher in the controls than in the total uRM group and the 2M, 3M and ≥4M subgroups. The level of vanadium was significantly lower in the controls than in the total uRM group (0.15 µg/L vs. 0.23 µg/L), and the level of lead was lower in the controls than that in the total uRM group and the 2M, 3M and ≥4M subgroups (0.01 µg/L vs. 0.28/0.18/0.63/0.34 µg/L). After adjusting for age, body mass index and education level, calcium and selenium exposure were consistently negatively associated with miscarriage, while lead exposure was positively associated with miscarriage. In addition, the correlations among exposures to different metals slightly differed between the control and uRM groups. Therefore, changes in some metal elements in the blood might be related to the risk of uRM.
A solid phase extraction-high-performance liquid chromatography-tandem Orbitrap high resolution mass spectrometry (HPLC-Orbitrap HRMS) method was established for the determination of 12 mycotoxins (ochratoxin A, ochratoxin B, aflatoxin B1, aflatoxin B2, aflatoxin G1, aflatoxin G2, HT-2 toxin, sterigmatocystin, diacetoxysciroenol, penicillic acid, mycophenolic acid, and citreoviridin) in edible oil, soy sauce, and bean sauce. Samples were extracted by 80:20 (v:v) acetonitrile-water solution, purified by PRiME HLB column, separated by aQ C18 column with mobile phase consisting of 0.5 mmol/L ammonium acetate-0.1% formic acid aqueous solution and methanol. The results showed that the limits of detection (LODs) and limits of quantification (LOQs) of 12 mycotoxins were 0.12–1.2 μg/L and 0.40–4.0 μg/L, respectively. The determination coefficients of 12 mycotoxins in the range of 0.20–100 μg/L were > 0.998. The average recoveries in soy sauce and bean sauce were 78.4–106.8%, and the relative standard deviations (RSDs) were 1.2–9.7% under three levels, including LOQ, 2× LOQ and 10 × LOQ. The average recoveries in edible oil were 78.3–115.6%, and the precision RSD (n = 6) was 0.9–8.6%. A total of 24 edible oils, soy sauce and bean sauce samples were analyzed by this method. AFB1, AFB2, sterigmatocystin and mycophenolic acid were detected in several samples at concentrations ranging from 1.0 to 22.1 μg/kg. The method is simple, sensitive, and rapid and can be used for screening and quantitative analysis of mycotoxin contamination in edible oil, soy sauce, and bean sauce.
该研究基于植物蛋白饮料掺杂使假现象普遍,建立一种针对榛子成分为检测目标的环介导等温扩增(Loop-mediated isothermal amplification,LAMP)快速检测技术方法.根据欧洲榛子染色体Ca8(登录号:LR899430.1)基因保守序列(第19517533~19519500 bp),设计榛子成分环介导等温扩增检测特异性引物,构建反应体系,并验证方法的特异性、灵敏度和稳定性;以Real-Time PCR(Polymerase Chain Reaction)为对照方法,采用显著性差异检验(McNemar's检验)方法,通过32种植物蛋白饮料检测结果验证LAMP方法的性能指标和准确性.该研究建立的LAMP方法特异性强,33种植物成分中除了榛子DNA外,其它植物成分DNA均未获得阳性扩增结果;重复性实验稳定性好(扩增Ct值,RSD=5.41%),最低检出限为0.1%(以质量分数计);通过植物蛋白饮料产品应用性验证,得出方法特异性和灵敏度均为100%,不存在假阳性和假阴性.综上,该研究建立的植物蛋白饮料榛子成分LAMP检测技术,具有操作简单、快速高效(从样品处理到最终结果可在2 h内完成)、准确度高等优点,可应用于植物蛋白饮料榛子成分快速检测.
The "Horsemeat Scandal " makes people pay more attention to the meat authenticity. However, expensive equipment, complicated operations, and professional personnel of current methods limit their field testing. In this study, CRISPR/Cas12a combined with recombinase polymerase amplification was used to establish a sensitive and rapid detection method for pig-derived component. The detection limit can reach to 10(-3) ng for pig DNA and be completed within 30 min. Beef and pork binary mixture models under different processing conditions of raw meat, boiled, and high-pressure were tested. Combining with two different DNA extraction methods, the detection limits of pork are as low as 0.1% and 0.001% (w/w), respectively. After 125 commercial products are tested, the results are completely consistent with the Chinese national standard real-time PCR method. This method not only has better detectability, but also can quickly and conveniently realize the visual identification of pig-derived ingredients, thus is suitable for on-site detection.