UPLC-MS/MS法同时测定外卖食品接触材料中7种抗氧化剂的迁移量

采用UPLC-MS/MS法，建立同时测定外卖食品接触材料中7种抗氧化剂迁移量的定量分析方法。结果表明：7种目标化合物在0.05～1.0 mg/L及0.5～10 mg/L范围内具有较好的线性关系，相关系数R2≥0.99；方法检出限为0.02～0.2mg/kg，定量限为0.05～0.5 mg/kg；方法的回收率为81.4%～116.1%，相对标准偏差为1.1%～9.8%。该方法前处理简单，灵敏度高，适用于外卖食品接触材料中抗氧化剂迁移量的定量分析。     

食品接触材料中壬基酚和辛基酚的测定与风险分析

目的研究食品接触材料中壬基酚和辛基酚的含量和迁移量的情况,并分析食品暴露风险。方法采用液相色谱-质谱联用法建立食品接触材料中壬基酚和辛基酚含量和迁移量的检测方法,并对相关检测数据进行统计分析。结果在优化条件下,壬基酚和辛基酚在5~200μg/L范围内线性关系良好,相关系数均大于0.999,壬基酚和辛基酚含量和迁移量的检测方法定量下限分别为0.1 mg/kg和10μg/kg,在添加水平为10,100,200μg/L时,样品中壬基酚和辛基酚含量的平均加标回收率为85.6%~89.2%,迁移量的回收率为94.3%~100.6%,相对标准偏差均小于15%。对30批次保鲜膜和复合包装袋样品进行检测,结果显示,6批次样品检出壬基酚或辛基酚,占总体样品的20%;其中1批次样品检出壬基酚迁移量,占阳性样品的16.7%。结论保鲜膜和复合包装袋可能含有壬基酚和辛基酚,且容易迁移到食品模拟物中,迁移量随着温度的升高和时间的延长而增加。保鲜膜和复合包装袋中的壬基酚和辛基酚存在一定风险,应引起足够重视。     

毛细管气相色谱法测定水杯密封垫圈中N-亚硝胺的迁移量

建立毛细管气相色谱法用于测定水杯密封垫圈中5种N-亚硝胺的迁移量。采用DB-5(30 m×0.53 mm,1.00μm)毛细管柱;程序升温:38℃保持4 min,以15℃/min的速率升至250℃保持4 min;N2为载气,流量为4.0 m L/min;氢火焰离子化检测器(FID),检测器温度为250℃;进样口温度为280℃;进样量为1.0μL。以2-叔丁基对甲酚为内标,通过内标对比法计算样品中5种N-亚硝胺的迁移量。在该色谱条件下,N-亚硝基二甲胺、N-亚硝基二乙胺、N-亚硝基吗啉、N-亚硝基哌啶和N-亚硝基二丁胺之间均能完全分离。此5种N-亚硝胺化合物分别在0.01~0.50,0.10~0.75,0.02~0.75,0.02~0.75,0.01~0.50 mg/kg的质量浓度范围内线性关系良好(r2=0.991 6~0.995 5);进样精密度(RSD)均小于5.0%(n=6);平均回收率为88.9%~96.7%(RSD5.0%,n=9)。定量限分别为0.01,0.10,0.02,0.02,0.01 mg/kg(信噪比为10∶1);检测限分别为2.0,20,2.0,2.0,2.0μg/kg(信噪比为3∶1)。采用本法测定3个厂家各2批水杯垫圈中N-亚硝胺的迁移量,均低于规定限度。该方法简便、准确、灵敏、重复性好、成本低,可用于水杯垫圈中N-亚硝胺迁移量的检测。     

啤酒易拉罐中苯酚和双酚A的迁移检测

目的建立一种测定啤酒易拉罐中苯酚和双酚A迁移量的方法,应用于市售易拉罐啤酒污染物的检测。方法选用体积分数为10%的乙醇为食品模拟物,在迁移温度为60℃,迁移时间为10 d的条件下开展迁移研究,采用高效液相色谱-荧光法对迁移样液进行检测。结果在文中的试验方法下,苯酚和双酚A在7 min内可实现完全分离,方法的检出限(LOD)分别为6.0和1.5μg/L。苯酚在20~400μg/L质量浓度范围内线性良好(相关系数为0.9999),双酚A在5~100μg/L质量浓度范围内线性良好(相关系数为0.9998)。通过对空白样品进行加标回收试验,苯酚回收率为90.0%~98.5%,相对标准偏差(RSD)为2.7%~6.2%;双酚A回收率为84.0%~102%,RSD为3.2%~5.3%。将该方法应用于7种易拉罐啤酒中苯酚和双酚A迁移量的检测,结果均未检出苯酚,双酚A检出量在6.9~14.8μg/kg之间。结论该方法准确度高、灵敏度好,能够满足啤酒易拉罐中苯酚和双酚A迁移量检测的要求。     

基于GC-MS/MS法测定食品包装纸中24种有害物质

目的 利用气相色谱串联质谱联用仪（GC-MS/MS）建立食品包装纸中24种有害物质（17种邻苯二甲酸酯（PAEs）和7种多氯联苯（PCBs））同时测定的方法。方法 样品处理后准确加入30 mL异丙醇和内标溶液,超声萃取40 min,使用气相色谱串联质谱仪进行检测,并采用内标法定量。结果 在0.02~1.0 μg/mL范围内,24种化合物的拟合曲线线性良好,相关系数R2在0.9945~1.0000之间,方法检出限和定量限分别为0.0005~0.0028 mg/L和0.0016~0.0089 mg/L,6种不同品牌的食品包装纸种的最高残留量为26.53 mg/kg。对24种化合物进行低、中、高3个水平浓度的加标回收试验,发现平均回收率在85.6%~109.7%之间,日内和日间的相对标准偏差分别小于6%（n=5）和9%（n=3）,回收率、重复性及精密度良好。结论 该方法简便、快速、结果准确可靠,适用于同时测定食品包装纸中24种有害物质,是一种高通量测试方法。     

GC法测定食品接触用再生PVC中氯乙烯类化合物的迁移量

目的 有效考察食品接触用再生聚氯乙烯类材料中氯乙烯、1,1-二氯乙烯和1,1-二氯乙烷的迁移风险。方法 建立测定食品接触用再生聚氯乙烯类材料中氯乙烯、1,1-二氯乙烯和1,1-二氯乙烷在水、酸性、含乙醇、橄榄油和化学替代溶剂中迁移量的气相色谱法。采用DB-624(60 m×250 μm×1.4 μm)毛细管柱对迁移实验后的3种物质进行组分分离，用电子捕获检测器(ECD)进行检测。结果 氯乙烯、1,1-二氯乙烯和1,1-二氯乙烷的色谱分离效果较好，在0.005~0.05 mg/kg内线性关系良好，检出限为0.001 mg/kg，定量限为0.005 mg/kg。当添加量为0.005、0.01和0.02 mg/kg时，3种物质的加标回收率为94.8%~108%，相对标准偏差(n=6)为0.0%~9.0%，均低于10%。结论 该方法具有较好的精密度和准确度，可用于食品接触用再生聚氯乙烯类材料中氯乙烯、1,1-二氯乙烯和1,1-二氯乙烷迁移量的测定。     

可降解包装材料中ATBC的迁移规律

目的 研究基于PLA/PBAT可生物降解食品保鲜袋中成分的测定,以及其中增塑剂乙酰柠檬酸三丁酯(ATBC)的迁移规律.方法 采用气相色谱-质谱联用仪检测材料中的成分及向食品模拟物中的迁移情况,并以此为基础,研究不同温度、不同厚度、不同时间、不同模拟物对ATBC迁移规律的影响;并采用红外光谱和扫描电镜从微观分析薄膜浸泡前后的变化.结果 在温度和厚度相同的条件下,ATBC在体积分数为95％的乙醇中迁移量最大;在同一种食品模拟物中,温度越高、时间越长,ATBC的迁移量越大;在温度和食品模拟物保持相同的条件下,厚度越小,ATBC的迁移量越大.结论 食品模拟物的性质、温度、厚度和时间都是影响ATBC迁移行为的重要因素.     

气相色谱-质谱法测定食品接触耐高温材料中氯苯和对二氯苯迁移量

目的利用气相色谱-质谱联用法测定食品接触耐高温材料中氯苯类物质(氯苯、对二氯苯等)的迁移量。方法从水基、酸性、醇类、油基等食品模拟物的迁移试验中得到的样品,通过正己烷或甲醇等有机溶剂萃取后,提取液中的氯苯类物质经由键合聚乙二醇的毛细管柱分离,最终在质谱中进行检测分析。结果在优化萃取溶剂、色谱柱等检测条件下,该方法可有效测定食品模拟物中氯苯、对二氯苯等物质的迁移量,在0.05~50 mg/kg(水性模拟物)或0.2~50 mg/kg(油性模拟物)的范围内线性良好,检出限可达到0.02 mg/kg(水性模拟物)或0.1 mg/kg(油性模拟物),回收率在87.6%~113.2%之间,相对标准偏差小于10%(n=6)。结论建立了食品接触材料中氯苯和对二氯苯迁移量的气相色谱-质谱联用方法,该方法简单、快捷、准确,满足了食品接触材料中氯苯类物质日常检验的要求。     

植物纤维增强聚乳酸发泡材料的研究进展

目的 建立基于电感耦合等离子质谱(ICP-MS)技术的总有机锡迁移量分析方法,用于食品接触材料中总有机锡的快速筛查。方法 使用四氢呋喃溶解法筛选出添加有机锡类热稳定剂的试样,采用水和体积分数为4%的乙酸模拟物进行迁移试验,迁移温度为20 ℃和40 ℃,迁移时间为10 d,同时比较常规浸泡迁移和超声加速迁移的结果,对检测方法的精密度、准确度进行了确认。结果 总有机锡迁移测定方法在质量浓度为0.13~13 μg/L时呈良好的线性关系,采用体积分数为4%的乙酸模拟物迁移的检出限为0.011 μg/L,定量限为0.033 μg/L;水模拟物迁移的检出限为0.0097 μg/L,定量限为0.029 μg/L。总有机锡加标回收率范围为98.1%~109.9%,相对标准偏差(RSD)<4.5%。结论 此方法具有灵敏度高、选择性好和准确性高等特点,适用于PVC包装材料中总有机锡迁移量快速分析。     

超高效液相色谱串联质谱法检测甘蔗中多种农药残留

针对甘蔗种植过程中常用的几种农药,采用分散固相萃取为前处理手段,建立了超高效液相色谱串联质谱法同时检测多菌灵、呋喃丹、乐果、敌敌畏、敌百虫的方法。甘蔗样品经粉碎后用乙腈超声提取,上清液经Qu EChERS方法净化后,采用UPLC-MS/MS法检测分析,外标法定量。结果表明,5种农药残留在1.0~50.0ng/m L的范围内具有良好的线性关系,其检出限为0.12~0.83μg/kg。方法的平均加标回收率为86.7%~106.8%,相对标准偏差为1.6%~4.3%(n=6)。该方法具有操作简单、快速高效、灵敏度高的优,能有效应对甘蔗种植过程中不同种类农药的同时检测。     

Insertion of triangulated surfaces into a meccano tetrahedral discretization by means of mesh refinement and optimization procedures

In this paper, we present a new method for inserting several triangulated surfaces into an existing tetrahedral mesh generated by the meccano method. The result is a conformal mesh where each inserted surface is approximated by a set of faces of the final tetrahedral mesh. First, the tetrahedral mesh is refined around the inserted surfaces to capture their geometric features. Second, each immersed surface is approximated by a set of faces from the tetrahedral mesh. Third, following a novel approach, the nodes of the approximated surfaces are mapped to the corresponding immersed surface. Fourth, we untangle and smooth the mesh by optimizing a regularized shape distortion measure for tetrahedral elements in which we move all the nodes of the mesh, restricting the movement of the edge and surface nodes along the corresponding entity they belong to. The refining process allows approximating the immersed surface for any initial meccano tetrahedral mesh. Moreover, the proposed projection method avoids computational expensive geometric projections. Finally, the applied simultaneous untangling and smoothing process delivers a high‐quality mesh and ensures that the immersed surfaces are interpolated. Several examples are presented to assess the properties of the proposed method.     

The Research of Anti-Wear Properties of Organomolybdenum Compounds in the Engine Oils

A four-ball tester was used to evaluate the anti-wear performance of three kinds of organomolybdemun compounds in the engine oils, i. e., molybdenum dialkyldithiophosphate (MoDDP), molybdenum dialkyldithiocarbamate ( MoDTC), and sulphur and phosphorus freeorganomolybdeum (Molybdate). The results indicate that a low concentration of MoDDP doesn' t improve the anti-wear properties of the commercial engine oils, but a high concentration of MoDDP can obviously improve the anti-wear properties and the load-carrying capacity of the engine oils. MoDTC doesn' t improve the antiwear properties of the engine oils, but worsens the anti-wear properties of the oils. Signifi can timprove ment of frictional and wear characteristics is obtained with Molybdate added in the commercial engine oils and the formulated oils.     

Certification Institutions Expected to Update and Transfer Information on Present Standards

Standards are the basis for production enterprises to organize production, ex-factory inspection, trade (delivery) and technical exchanges, product certification, quality arbitration and supervision.……     

Flow calorimeter for enthalpy increment measurements on condensed gases

A flow calorimeter for enthalpy increment measurements on condensed gases is presented. A better knowledge of the properties of the liquefied natural gas is needed, and therefore a liquid loop has been designed for our flow calorimeter. The fluid loop in the calorimeter is designed in order to avoid the two-phase region, since two phases would give compositional disturbances in the measurements. The avoidance of the two-phase region is made possible by increasing the pressure of the test fluid after the measurement section, then heating the fluid at super-critical pressure past the critical point. Finally, the fluid is throttled to the low-pressure gas state at the inlet condition of the compressor that circulates the fluid. To perform the pressure increase, a new cryogenic pump has been designed. To evaluate the new equipment, measurements were taken on liquid ethane over the temperature range 146–256 K at pressure between 0.9 and 5.1 MPa.     

Refrigerators Enter a New Era of Health Preservation Frestech initiates the establishment of China's first standard for household sterilization refrigerators

On November 30, 2007, the China Association for Standardization (CAS) held a press conference at Beijing Diaoyutai State Guest House. Leaders from the China Household Electric Appliance Research Institute, the China Household Electric Appliance Association, and the China Consumers' Association attended and made speeches.……     

Optimum-Simulation von Ernteprozessen

Zusammenfassung Bei der Gestaltung von Ernteprozessen — beispielsweise des Prozesses Mähdrusch, Körnertransport und -abnahme — als transportverbundene Fließarbeitsverfahren mit mindestens zwei verschiedenen Arbeitsmitteln gibt es einen großen Optimierungsspielraum. Solche Prozesse sind mehrstufige Bedienungsprozesse mit gemischter Anordnung der Bedienungseinrichtungen. Außerdem besitzen sie stark ausgeprägte räumliche Aspekte. Es wird vor allem gezeigt, welche Merkmale solcher Prozesse in Simulationsmodellen abgebildet sein müssen, welche Zielgrößen in Abhängigkeit von welchen Einflußgrößen unter Berücksichtigung welcher Prozeßbedingungen ermittelt werden sollten und wie der Bewertungsprozeß zur Ermittlung der gewünschten Informationen gestaltet werden muß.     

A study of centrifugal cast high boron high speed steel

In the present study a high‐boron high speed steel (HSS) roll material was designed. Many expensive alloy elements have been substituted by cheap boron alloy, and high‐boron high speed steel roll has been manufactured by centrifugal casting method. The microstructures, mechanical properties and wear resistance of centrifugal casting high‐boron high speed steel roll have been investigated by optical microscopy (OM), scanning electron microscopy (SEM), and X‐ray diffraction (XRD) analysis, hardness test, impact test and wear test. The results indicated that the solidification microstructures of high‐boron high speed steel roll consisted of M₂(B,C), (W,Mo)₂(B,C), M₃(B,C), M₂₃(B,C)₆ type borocarbides and martensite, a small amount of retained austenite. Borocarbides were continuously distributed over the grain boundary. After quenching from 1050 °C, local broken network appeared in partial borocarbides, and fine secondary borocarbide precipitated from the matrix. After tempering from 525 °C, the amount of precipitated borocarbide increased significantly. After heat treatment, the hardness of high‐boron high speed steel roll excelled 60 HRC, and its impact toughness excelled 8.0 J/cm². The single groove steel rolling amount of high‐boron high speed steel rolls increases by 500% than that of bainite cast iron roll, when the rolls are used in K₁ mill housing of bar mill.     

Certification Becomes Important for the I Quality; and Safety Supervision of the Chinese Liquor Sector

The end of 2007, over 200 unit products of more than 80 Chinese firms have passed the quality grade certification for liquor products. These products involve distilled spirits, beer, wine, yellow wine, fruit syrup wine and others, and cover over 80% of the national top-branded liquor products.……     

Deposition and Coating Properties on CVD Tungsten

Surface characterization and microstructure studies are performed on chemical vapor deposited (CVD) tungsten coating. There is about 2 μm thickness diffusion layer of tungsten in the molybdenum substrate. The thermal shock test shows tungsten coating has good adhesion with molybdenum substrate, but the elements of oxygen and carbon in the tungsten coating have the bad affection to the adhesion. The result of high-temperature diffusion experiment is the diffusion rate from molybdenum substrate to tungsten coating is faster.