A novel malachite green molecularly imprinted membrane (MG-MIM) with specific selectivity for malachite green (MG) and leucomalachite green (LMG) was prepared using a hydrophobic glass fiber membrane as the polymer substrate, methyl violet as a template analog, 4-vinyl benzoic acid as the functional monomer, and ethyleneglycol dimethacrylate as the crosslinking agent. MG-MIM and non-imprinted membrane (NIM) were structurally characterized using scanning electron microscopy, surface area analyzer, Fourier-transform infrared spectrometer and synchronous thermal analyzer. The results showed that MG-MIM possessed a fluffier surface, porous and looser structure, and had good thermal stability. Adsorption properties of MG-MIM were investigated under optimal conditions, and adsorption equilibrium was reached in 20 min. The saturated adsorption capacities for MG and LMG were 24.25 ng·cm−2 and 13.40 ng·cm−2, and the maximum imprinting factors were 2.41 and 3.20, respectively. Issues such as “template leakage” and “embedding” were resolved. The specific recognition ability for the targets was good and the adsorption capacity was stable even after five cycles. The proposed method was successfully applied for the detection of MG and LMG in real samples, and it showed good linear correlation in the range of 0 to 10.0 μg·L−1 (R2 = 0.9991 and 0.9982), and high detection sensitivity (detection limits of MG and LMG of 0.005 μg/kg and 0.02 μg·kg−1 in shrimp, and 0.005 μg/kg and 0.02 μg/kg in fish sample). The recoveries and relative standard deviations were in the range of 76.31–93.26% and 0.73–3.72%, respectively. The proposed method provides a simple, efficient and promising alternative for monitoring MG and LMG in aquatic products.

建立鸡蛋样品中那西肽的高效液相色谱-串联质谱检测方法.样品经甲酸-乙腈溶液提取后,正己烷除脂,再经HLB固相萃取柱净化;样品溶液通过高效液相色谱-串联质谱进行检测,采用负离子模式电喷雾电离,配合多反应离子扫描分析目标化合物.分别对样品前处理条件及色谱质谱参数进行优化.结果表明,采用1％甲酸-乙腈溶液萃取,经HLB固相萃取净化,定容液用聚四氟乙烯滤膜过滤,以醋酸铵-乙腈作为流动相,能够实现那西肽的快速测定.在优化条件下采用基质标准曲线外标法定量分析,那西肽在1.0～20.0 μg/L质量浓度范围内线性关系良好,相关系数R2大于0.998,方法的检出限为0.3μg/kg,定量限为1.0μg/kg.在1.0、2.0 μg/kg和10 μg/kg添加量下,那西肽的平均回收率为83.8％～96.2％,相对标准偏差为6.0％～8.8％.该方法简便快速、灵敏度高、准确性好,适用于鸡蛋中那西肽残留的监测.

Because only very weak signals of fragment ions of nosiheptide can be obtained, nosiheptide is usually detected by liquid chromatography-tandem mass spectrometry (LC-MS/MS) via the determination of its hydrolyzed degradation product named HMIA in previous studies. The indirect method suffers from several problems, such as complicated samplepreparation, unavailable commercial HMIA, and the risk of the false-positive result by HMIA. However, we found that nosiheptide could produce several significant fragment ions under high collision energy (CE). Therefore, we developed a method for the direct determination of nosiheptide by LC-MS/MS in animal tissues. The sample was extracted with ACN, then degreased with n-hexane, and purified by an HLB solid-phase extraction (SPE) cartridge. After being filtered through the PTFE filter, it was analyzed by LC-MS/MS in selected reaction monitoring (SRM) mode. The influencing factors, such as mobile phase, SPE cartridge, filter material, and matrix effect, were investigated. Nosiheptide showed a good linear relationship (R2 ≥ 0.999) within the concentration range from 0.3 μg/L to 20 μg/L under optimized conditions. The limit of detection (LOD) was 0.3 μg/kg, while the limit of quantification (LOQ) was 1.0 μg/kg in chicken, bovine muscle, swine muscle, and swine liver. The average recoveries at spiked levels of 1.0, 2.0, and 10 μg/kg ranged from 83% to 101%, with the relative standard deviations (RSDs) <12%. Compared with the methods previously reported, our newly developed method was more simple, convenient, and sensitive. Moreover, it was successfully applied for the determination of nosiheptide residue in medicated chicken samples.

Correction for ‘Determining the geographical origin of milk by multivariate analysis based on stable isotope ratios, elements and fatty acids’ by Siyan Xu et al., Anal. Methods, 2021, DOI: 10.1039/d1ay00339a.

食品的营养标签通过向消费者直接展示产品特性,引导消费者合理选择食品,标签准确规范才能保证消费者不受误导.本文对预包装食品营养标签标示常见问题进行汇总与分析,提高预包装食品营养标签标示水平,保护消费者合法权益.

To construct a reliable discrimination model for determining milk geographical origin, stable isotope ratios including δ13C, δ15N and δ18O, 51 elements and 35 fatty acids (FAs) in milk samples from Australia, New Zealand and Austria were detected and analyzed. It is found that all of the stable isotope ratios in the milk samples of Australia are the highest, followed by those of the samples from New Zealand and Austria. In addition, 14 elements and 8 FAs show different contents in the samples of different countries at the significance level of P < 0.05. Based on these results, a multivariate model with good robustness and predictive ability for authenticating milk origin (R2X = 0.693, Q2 = 0.854) was successfully constructed. Element contents and stable isotope ratios are more reliable variables for milk origin discrimination and Rb, δ18O, Tl, Ba, Mo, Sr, δ15N, Cs, As, Eu, C20:4n6, Sc, C13:0, K, Ca and C16:1n7 are the critical markers in the multivariate model for verifying milk origin.

A novel method for hierarchical screening of illegal adulterants in Fur seal ginseng pills (FSGP) products was developed by microwave-assisted extraction (MAE) coupled to salting-out assisted liquid-liquid extraction (SALLE) with multi-dimensional fingerprint profiling analysis. Using a homogeneous system formed by dimethyl carbonate (DMC) and water as the extractant, the MAE conditions were investigated to maximize extraction recoveries, followed by addition of ammonium sulfate to induce DMC phase separation for SALLE enrichment of 16 potentially illegal adulterants such as phosphodiesterase type-5 inhibitors, androgens, α receptor antagonists and yohimbine etc. By means of high-performance liquid chromatography (HPLC) with diode array detection (DAD) and fluorescence detection (FLD), multi-dimensional fingerprints were acquired by multi-wavelength detection to highlight the signals of the potentially illegal adulterants and reduce or remove interferences from the sample matrix. For high accuracy and reliability, a hierarchical screening strategy was designed by multi-dimensional fingerprinting profiling analysis (MDFPA). The method exhibited proper identification and quantification performance, and it was successfully applied to screening of illegal adulterants in 18 batches of the samples through the step-by-step MDFPA. Also, the results were further confirmed by ultra high-performance liquid chromatography-quadrupole-orbitrap mass spectrometry (UHPLC-Q-Orbitrap/MS). The proposed method was proved to be a green, efficient and reliable alternative to monitoring aphrodisiac health products.

本文译自国际食品法典委员会"CAC/GL 90-2017食品和饲料中农药残留分析方法性能标准指南".该指南规定了农药残留分析方法的选择和验证原则、分析方法的性能参数、筛选方法的性能指标、定量方法的性能指标、分析物鉴定方法和确证方法的性能标准和定义等.本译文可为我国食品和饲料中农药残留分析专业人员研发和验证化学分析方法或与国外检测机构交流提供参考.

A novel, efficient and specific aptamer-functionalized sorbent was successfully synthesized and applied in the analysis of ultra-trace aflatoxin M1 (AFM1) and its analogues in milk. By using a gold nanoparticle-based colorimetric analysis tool, we could determine that the AFM1-aptamer (M1-aptamer) recognized and bound AFM1 to generate an aptamer-target complex. After analysis and verification, the M1-aptamer on the surface of the carboxyl microspheres were completely modified via EDC/NHs amide formation. The effects of extraction pH, extraction buffer, concentration of Mg2+ and elution solvents were investigated by single-factor experiments to determine the most suitable analysis conditions. Using these conditions, the extraction performance of the M1aptamer-functionalized sorbent could be studied and an analytical method for AFM1 and its analogues in milk could be established. The results of adsorption equilibrium as well as adsorption selectivity experiments indicated that the M1-aptamer offered a specific adsorption site to selectively adsorb aflatoxins exhibiting a dihydrofuran oxaphthalene scaffold. The adsorption capacity of the aptamer-functionalized sorbent was 233.1 mu g/g. A studied method for the determination AFM1 in milk with low matrix effect demonstrated a good linear correlation in the range of 0 to 2.0 mu g/L (R2 = 0.9982) and high detection sensitivity (detection limits of 7 ng/kg in milk and 21 ng/kg in milk power). Furthermore, excellent spiked recovery and good repeatability were obtained. The method delivered specific, accurate and reproducible results for enriching and detecting ultra-trace AFM1 and its analogues in milk.

采用液相色谱-串联质谱法对畜禽表皮组织中的松香酸和脱氢松香酸含量进行检测.样品中的松香酸和脱氢松香酸用乙腈提取,经HLB固相萃取柱净化,采用液相色谱-串联质谱进行检测.色谱柱:反相C18柱(100 mm×2.1 mm,2μm);流动相:0.1％甲酸溶液和0.1％甲酸-甲醇溶液(10∶90,V/V);流速:0.3 mL/min;质谱分析采用电喷雾电离正离子模式检测,扫描方式为多反应监测.结果 表明:松香酸线性范围为2.0～100 μg/L,检出限为1.1 μg/kg,定量限为3.6 μg/kg;脱氢松香酸线性范围为5.0～250 μg/L,检出限为3.9 μg/kg,定量限为13 μg/kg.在5.0～200 μg/kg添加量范围内松香酸和脱氢松香酸的回收率为81.7％～93.7％,相对标准偏差均在12％以内.方法 用于实际样品分析,多个畜禽表皮样品中检出松香酸及脱氢松香酸,采用松香甘油酯进行脱毛的鸭皮中也检出了一定含量的松香酸及脱氢松香酸.本实验建立的分析方法简便快捷,具有较好的灵敏度和可靠性,可用于畜禽表皮组织中松香酸和脱氢松香酸的定量确证分析.

The analysis of mycotoxins in foodstuffs is affected by the complexity of the matrix and the extremely low concentration levels. The development of sample pretreatment and analytical methods that enable highly selective enrichment as well as highly sensitive detection is of great significance for food safety. This paper reviews the recent progress in biotoxin analysis methods and summarizes the prospects and development of this field.

预包装食品标签是消费者选购食品时了解食品信息的重要途径,准确的食品标签才能保障消费者合法权益.进口预包装食品标签检验作为进口食品检验监管的重要要素之一,在进口食品检验监管中占有重要地位.本文对我国进口预包装食品标签检验中的一些关键要素及常见问题进行了总结,以期对进口预包装食品标签检验有所帮助.

食品标签是进口预包装食品检验的重要内容之一.为了响应进口预包装标签检验监管最新要求,本文汇总了进口预包装食品标签常用相关法律法规标准,总结了进口预包装食品标签设计和检验中一些容易忽视的问题并进行了分析,包括未使用规范汉字、食品名称与其他标准规定的名称冲突、配料中食品添加剂标示不规范、字符高度不满足要求、没有关注到包装内产品的情况、生产日期、保质期顺序与标示顺序不一致、营养标签标示不规范等,希望对进口预包装食品标签的设计和检验有所帮助.

我国进口食品种类和数量的不断增加, 加剧了进口食品安全监管的复杂性.我国进口食品安全监管要求日益完善, 目前的监管要求主要有:进出口商备案、检疫审批及准入、境外生产企业注册、提供相关证书以及依照食品安全国家标准检验等.但在实际监管中仍存在一些问题, 包括伪报食品属性逃避特殊监管要求、食品配料信息不准确增加监管风险、预包装食品标签检验与监管衔接不畅增加监管风险、标准体系不完善等,本文对这些问题进行了分析并提出了改进建议, 以期对进口食品检验监管有所帮助, 促进进口食品健康发展,保障进口食品安全.

A novel method for screening and quantification of illegal adulterated antidiabetics in hypoglycemic health products was developed by multi-dimensional fingerprint profiling analysis (MDFPA). By means of aqueous two-phase extraction (ATPE), using aqueous two-phase system (ATPS) of butanol-water as the extractant, 11 common antidiabetics could be effectively extracted to the upper and lower phases, respectively. HPLC separation conditions for the extracts from two phases were investigated by multi-wavelength detection before and after p-nitrobenzoyl chloride (p-NBC) and 2,4-dinitrofluorobenzene (DNBF) derivatizations to establish multi-dimensional fingerprints. For high accuracy and reliability, a hierarchical screening approach to screening illegal adulterated antidiabetics in samples was established by MDFPA and spectral purity examination. Meanwhile, detection limits of identification for illegal adulterants were defined by detection limits of spectra (SLOD). The proposed method exhibited good identification and quantification performances. SLODs, LODs and LOQs of 11 antidiabetics were 1.22-8.37 mu g/g, 0.225-4.23 mu g/g and 0.755-14.10 mu g/g, respectively. They had good linearity ranged from 2.0 mu g/g to 300.0 mu g/g (R-2 >= 0.9978). The recoveries and RSDs were 76.83-109.6% and 0.50-6.5%, respectively. The method was successfully applied to screening of 15 batches of samples in different forms. Among them, four samples were detected to contain 5.47 mu g/g of metformin, 6.50 mu g/g of phenformin, 3.69 mu g/g of glibenclamide and 9.11 mu g/g of glimepiride, respectively. The results proved that it was an efficient and feasible alternative to screening and detection of illegal adulterated antidiabetics in hypoglycemic health products. (C) 2020 Elsevier B.V. All rights reserved.

本项目以食品中化学性有害物为研究目标,阐明了182种化学性有害物的质谱软电离裂解机理,在质谱检测机理方面取得突破;针对化学性有害物发掘技术缺失的问题,开创了基于标志性中性丢失/碎片质谱扫描的发掘技术;开发了高选择性富集材料、试剂和设备,实现了检测灵敏度、特异性、准确度、重复性、再现性和速度的显著提升.该项目研发的质谱软电离裂解机理、有害物发掘技术、精准检测等关键技术达到国际先进水平,在应对“供港生猪瘦肉精”“臭脚盐”“输欧牛肝菌尼古丁”等突发事件中发挥了关键作用,有效支撑了科学监管,增强了我国进出口食品安全监管科技水平和技术能力,取得了显著的经济和社会效益.

A method for screening illegal adulterated antidiabetics in bitter melon and ginseng soft gels (BMGSG) was developed by multi-fingerprinting profiling analysis. HPLC fingerprints of BMGSG samples were investigated for chemical feature and similarity evaluation. Based on chemical structure and spectroscopic properties, chromatographic behaviors of common antidiabetics were further studied under different HPLC conditions combining with multi-wavelength monitoring with diode array detector (DAD) and fluorescence detector (FLD) to highlight and discriminate illegal adulterants in BMGSG products. Thereby, a hierarchical strategy for screening illegal adulterated antidiabetics was designed by multi-fingerprinting profiling analysis coupled to spectral purity examination. Detection limit of identification (ILOD) and detection limit of spectra (SLOD) were defined in the range of 0.115–2.65 μg/mL and 0.382–2.72 μg/mL, respectively. The method also demonstrated good quantification performance through validation tests. It had been successfully applied to screening real samples, and the results were confirmed by ultra-performance liquid chromatography-quadrupole-orbitrap mass spectrometer (UPLC-Q-Orbitrap/MS). Thus, the proposed method was an efficient and reliable approach for detection of illegal adulterated antidiabetics in the dietary supplement.

(1.上海出入境检验检疫局动植物与食品检验检疫技术中心,上海 200135) (2.深圳出入境检验检疫局食品检验检疫技术中心,广东深圳 518045)(3.上海大学生命科学学院,上海 200444) 摘要:建立了黄油中雌酮、α/β-雌二醇、雌三醇和孕酮 5 种类固醇激素的气相色谱/燃烧炉/同位素比质谱(GC/C/IRMS)溯源方 法。样品经乙酸乙酯-环己烷(1:1,V/V)提取,经凝胶渗透色谱(GPC)净化和半制备液相色谱(Pre-HPLC)纯化,纯化液经 HP-5MS (30 m×0.25 mm,0.25 μm)柱分离,GC/C/IRMS 溯源分析和气相色谱-质谱(GC/MS)定性和定量分析。黄油中外源性激素 δC 值 <-30‰,内源性激素 δC 值>-27‰,其中黄油中外源性孕酮 δC 值=-30.59‰±0.12‰,内源性孕酮 δC 值范围在-26.83‰±0.25‰与 -23.80‰±0.33‰之间,单因素方差分析(p 值=0.009<0.05)显示内源性孕酮和外源性孕酮的 δC 值存在显著差异性。经模拟实验显

A novel method for hierarchical screening of illegal adulterants in Fur seal ginseng pills products was developed by multi- dimensional fingerprint profiling analysis. Fingerprint feature of the samples was acquired by high- performance liquid chromatography analysis of 11 batches of samples with diode array detector and fluorescence detector, and then potential illegal adulterants including phosphodiesterase type- 5 inhibitors, androgens, a receptor antagonists and yohimbine, were further separated at multiple wavelengths to reduce or remove interferences from sample matrix for highlight their chromatographic characteristics. Accordingly, a hierarchical screening strategy was designed by first- order and second- order fingerprints combined with spectral examination to achieve high accuracy and reliability. The method was successfully applied to screening of illegal adulterants in real samples, and it also exhibited good quantification performance through validation tests. From 16 batches of samples, three suspected samples were confirmed to be positive, containing 9.37 mu g/g of testosterone, 18.8 mu g/g of tadalafil, and 48.5 mu g/g of sildenafil, respectively. The recoveries and relative standard deviations were in the range of 83.6-103.1% and 4.2-6.8%, respectively. The proposed method provided a simple, efficient and promising alternative to monitoring functional foods.

The safety of cosmetics attributing to the illegal addition of antibiotics for quick effect is a big concern nowadays. Nitrofurans, one of commonly added illegal antibiotics, are strictly banned in cosmetics in China. It is still a great challenge for the rapid and precise analysis of trace nitrofurans when facing various cosmetics with complicated matrices. Surface-enhanced Raman spectroscopy (SERS) is emerging as a novel rapid on-site analytical technique. In this work, an accurate SERS method was developed for the rapid analysis of trace nitrofurantoin in various cosmetics by use of nanoarrayed hydroxyl polystyrene (PS-OH)-based substrate. A series of characterizations indicated the successful synthesis of Au@PS-OH substrate and the uniform distribution of gold nanoparticles on the substrate surface. The SERS substrate revealed good selectivity and reproducibility with an enhancement factor of 2.6x10(4). Finally, an analytical method for the determination of nitrofurantoin in cosmetics was established by SERS using Au@PS-OH substrate coupling with efficient sample preparation process. It was satisfied that trace nitrofurantoin could be actually detected and quantified to be 1.77 and 7.74 mg/L in a mouthwash and rose-mist sample, respectively, with good recoveries of 86.8-106% and relative standard deviations of 0.9-2.9%. The comparable analytical results for real samples were achieved by the traditional high-performance liquid chromatography (HPLC) method, which validated the reliability of the proposed method. It is expected that this SERS method has great potential for the rapid and on-site analysis of trace additives in cosmetics.