Rapid screening and quantification of cyromazine,melamine, ammelide,ammeline, cyanuric acid,and dicyandiamide in infant formula by ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry and triple quadrupole mass spectrometry

In the past few years, special concern for triazine pesticide cyromazine (CYRO) and its metabolites melamine (MM), ammelide (AMD), ammeline (AMN), cyanuric acid (CA), and dicyandiamide (DCD) residues has arisen in the food safety field on infant foods. In this work, screening and confirmation for infant milk powder samples were performed by quadrupole time-of-flight mass spectrometry (QTOF-MS). An accurate mass database was established. The matrix-matched internal standard calibration curves of UPLC–MS/MS were linear, with correlation coefficient (r²) higher than 0.994. The limits of quantification (LOQ) were 1.6, 5.0, 16.5, 10.0, 66.4, and 66.4 μg/kg for CYRO, MM, AMD, AMN, CA, and DCD, respectively. The average recoveries ranged from 64.8 to 103%. The retention time, intra- and inter-day precisions (relative standard deviation, RSDs) of 6 analytes were in the range of 0.02–0.05%, 2.4–6.1%, and 7.2–11.2%, respectively. CYRO and MM residues in some infant milk powder samples were confirmed. Quantitation of positive samples was performed using the internal standard method and six-point matrix-matched calibration curves. The content for CYRO in all 8 samples and MM in 4 samples were in the range of 3.5–45 μg/kg and 8–25 μg/kg, respectively. The method developed for the first time has high sensitivity, can be used as an effective tool for rapid screening and highly sensitive multiresidue determination of CYRO, MM and their metabolites AMD, AMN, and CA as well as DCD in milk powder samples.     

甲萘威在棉花和土壤中的残留和消解动态

采用液相色谱-串联质谱法(LC-MS/MS)研究了甲萘威在棉花和土壤中的残留消解动态,为棉花上甲萘威的安全使用提供科学依据。样品经甲醇+二氯甲烷(体积比1∶99)提取,氨基固相萃取柱净化,后经LC-MS/MS测定其残留量。甲萘威在棉叶上的半衰期为1.1~1.9 d;在土壤中的半衰期为4.3~6.2 d。试验条件下,甲萘威在收获前14 d、收获前7 d、收获期棉籽中的残留量≤0.023 mg/kg。建议30%聚醛·甲萘威颗粒剂在推荐剂量下最多施药1次,采收间隔期为7 d。     

Duplex PCR approach for the detection and quantification of donkey,horse and mule in raw and heat‐processed meat products

Donkey‐related products have been paid more attention for their high nutritional value to human beings. Due to donkey resource scarcity, coupled with gradually increasing market demand, adulterated donkey meat products with other low‐cost animal meat, especially with the similar species horse and mule, are often found in market. Therefore, detection of species fraud in donkey meat products is important for consumer protection and food industries. In this study, a simple and highly specific duplex PCR method, based on the simultaneous amplification of fragments of the mitochondrial ATP synthase subunit 8/6 and ND2, was developed and optimised for the identification of horse, donkey and mule species in raw and heat‐processed meat products. To the best of our knowledge, it was the first time for this strategy applied to these three genetically related animal meat products differentiation to date. The duplex PCR generated a 153‐bp and 83‐bp amplification products for horse and donkey, respectively. While for mule, both of the two length amplification products are appeared on the agarose gel. Target meat species could be detected at a level of 1%, and the results indicated that the duplex PCR assay could be used in the authentification of donkey‐related products with high specificity, cost‐effectiveness and simplicity.     

高效液相色谱-氢化物发生-原子荧光光谱联用技术测定富硒大米中的5种硒形态

目的建立高效液相色谱-氢化物发生-原子荧光光谱法(high performance liquid chromatographyhydride generation-atomic fluorescence spectrometry,HPLC-HG-AFS)检测富硒大米中硒代胱氨酸(Se Cys2)、甲基硒代半胱氨酸(Me Se Cys)、亚硒酸根(Se IV)、硒代蛋氨酸(Se Met)和硒酸根(Se VI)的方法。方法选择Hamilton PRP-X100阴离子交换色谱柱,对流动相浓度、p H值以及提取条件进行选择优化。样品采用链霉蛋白酶E水解超声提取方式,使用40 mmol/L的磷酸氢二铵溶液(p H 6.0)作为流动相。结果 20 min内可以完全分离5种硒形态,各种硒形态标准曲线线性相关系数(r)均大于0.999,检出限分别为3.7、1.7、1.2、4.2、7.2μg/L。加标回收实验显示富硒大米中硒的主要存在形态即硒代蛋氨酸回收率范围在95.1%~98.2%,其他4种硒形态回收率范围均在80.4%~102.5%。结论本方法可以快速、准确地测定大米中硒的5种形态。     

杜马斯燃烧法测定油料作物中粗蛋白质含量的 方法优化及其与凯氏定氮法的比较研究

目的建立杜马斯燃烧法测定油料作物中粗蛋白质含量的方法,并与凯氏定氮法进行比较。方法以芝麻、大豆、油菜和花生为研究对象,对杜马斯燃烧法的称样量和氧气系数进行优化。分别用杜马斯燃烧法和凯氏定氮法测定4种样品的粗蛋白含量,并对2种测试方法的结果进行比较分析。结果杜马斯燃烧法的测定值略高于凯氏定氮法,但2种方法的测定值间没有显著性差异(P0.05),杜马斯燃烧法比凯氏定氮法的测定精密度和准确度更高。测定结果的相关性分析表明两种方法的测定值呈显著相关(r~2=0.9988)。结论杜马斯燃烧法的精密度和准确度更好,可以替代凯氏定氮法测定油料作物的粗蛋白质含量。     

Development of a rapid magnetic bead-based immunoassay for sensitive detection of zearalenone

Here we demonstrate a novel magnetic bead-based enzyme-linked immunosorbent assay (MB-ELISA) for zearalenone (ZEN) detection. Firstly, an anti-ZEN monoclonal antibody (mAb) was prepared by hybridoma technique, and immobilized on carboxyl modified MBs to obtain mAb-MBs. In addition, the biotinylated ZEN-BSA was labelled by streptavidin-HRP for use as competitor. Based on the mAb-MBs and streptavidin-HRP labelled ZEN-BSA, a MB-ELISA which contains only one 20 min antigen-antibody reaction step and takes no more than 45 min for dozens of samples analysis was developed. The half maximal inhibitory concentration (IC₅₀) and limit of detection (LOD) of the MB-ELISA are 1.78 ng/mL and 0.13 ng/mL, respectively. And the MB-ELISA working range for corn samples analysis is from 5.0 μg/kg to 255.2 μg/kg. The recoveries for ZEN spiked corn samples ranged from 82.3 to 110.5% with coefficient of variation (CV) under 8.9%. For natural corn samples analysis, the results of MB-ELISA showed good agreement with the results of conventional direct competitive ELISA (R² = 0.9742).     

基于荧光探针的汞离子检测方法研究

目的建立基于荧光探针的汞离子快速检测方法。方法基于汞离子促进硫羰基脱硫的不可逆反应,设计合成了含有双硫羰基的荧光探针HgP1。通过紫外-可见光谱法和荧光光谱法研究了探针HgP1在甲醇水溶液中对金属离子的识别特性,并探讨了其识别机制。结果探针HgP1对Hg~(2+)具有高效专一的选择性,具有较强的抗金属阳离子和阴离子干扰能力,并能通过溶液颜色变化实现对汞离子的裸眼识别。Hg~(2+)浓度在0.01~0.1μmol/L范围内与该探针溶液荧光发射强度值间呈良好的线性关系(R~2=0.988),该方法对汞离子的最低检测限为0.256μg/kg。结论 HgP1探针对汞离子具有高效专一的选择性,其最低检测限满足国家标准对食品中汞离子的限量要求,具备较强的实际应用价值。