蒸汽萃取-高效液相色谱紫外/荧光法同时测定果蔬中噻苯咪唑、邻苯基苯酚、联苯及抑霉唑残留

建立了一种快速同时测定果蔬中噻苯咪唑（TBZ）、邻苯基苯酚（OPP）、联苯（DP）及抑霉唑（IMZ）残留量的高效液相色谱紫外/荧光分析方法。柑橘类水果及蔬菜样品经组织捣碎机打碎研磨均匀后,利用咖啡萃取机产生的甲醇或乙醇蒸汽进行萃取,分别采用紫外/荧光检测器同时测定上述四种或三种防腐保鲜剂。结果表明：紫外检测TBZ、OP...     

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。     

磁性多壁碳纳米管固相萃取-气相色谱质谱联用快速测定食用油中的苯并[a]芘

建立以磁性多壁碳纳米管(Fe3O4/MWCNTs)作为磁固相萃取吸附剂,气相色谱-质谱联用检测食用油中苯并[a]芘(Ba P)的方法。实验优化萃取时间、洗脱溶剂的种类和用量、洗脱时间等影响萃取效率的主要参数。最佳样品处理条件为:萃取时间5 min、4 m L甲苯作为洗脱剂超声洗脱3 min。在最佳条件下,该方法具有较高的准确性和灵敏度,其回收率为95.3%~100.5%,检出限(3倍信噪比)为0.15μg/L。检测市售食用油中的Ba P时,实际样品加标回收率为77.2%~89.1%,相对标准偏差为1.1%~6.0%,检出限为0.19%~0.29μg/L,该方法操作简便、耗时短、有毒试剂用量少、准确灵敏。     

固相萃取-超高效液相色谱质谱联用法测定水产品中左氧氟沙星残留

建立了水产品中左氧氟沙星残留的超高效液相色谱串联质谱检测法。采用乙腈对样品中的待测物进行提取,正已烷除脂,浓缩后用固相萃取小柱进行净化,吹氮浓缩后采用超高效液相色谱质谱联用-电喷雾正离子和MRM多反应监测模式进行定性定量分析。检测浓度线性范围为0～100μg/kg,线性相关系数为0.9922,检出限为4.5μg/kg。在鳗鱼、虾和罗非鱼三种不同样品基质中进行添加浓度为10,20,50μg/kg的验证试验,该药物的回收率在72.5%～83.5%内,相对标准偏差(n=6)在7.9～11.4%之间,并对其质谱裂解和基质效应进行了研究。本检测方法快速,高效,灵敏度高,符合检测要求。     

气相色谱-质谱联用法测定印制线路板中多溴联苯及多溴联苯醚的不确定度评估

分析了气相色谱-质谱联用法测定印制线路板中多溴联苯(PBBs)及多溴联苯醚(PBDEs)含量的不确定度来源,求出各不确定度分量,将不确定度分量合成给出实验结果不确定度。     

固相萃取-气相色谱-质谱联用法检测进出口蔬菜产品中百菌清残留

建立了固相萃取-气相色谱-质谱法检测蔬菜中百菌清残留的分析方法。样品用乙腈-水-磷酸混合液提取,经液液分配、Florisil/Na2SO4柱净化后过滤膜上机。采用选择离子扫描方式,外标法定量。通过优化前处理和上机条件,在最优条件下进行测试,实验结果百菌清的定量检出限为0.001mg/kg,在加标水平0.005～0.1mg/kg范围内,回收率为78.65%～90.67%,相对标准偏差为3.5%～5.8%。该方法简便、快速、净化效果理想,能满足残留分析的要求,可用于进出口蔬菜中百菌清残留的检测。     

高效液相色谱法检测食品接触材料中三聚氰胺的残留量

建立了一种用液相色谱技术检测分析食品接触材料中三聚氰胺残留量的方法。样品采用0.1 mol/L盐酸作为提取溶液,70℃水浴超声提取。色谱分离采用NH2柱,流动相为V(乙腈):V(5mmol/L磷酸盐缓冲溶液,pH 6.5)=75:25,二极管阵列检测器检测。在优化条件下,三聚氰胺浓度在0.2-100 mg/L范围内与其峰面积线性关系良好,检出限(S/N=3)为0.02 mg/L。在100μg的添加水平下,三聚氰胺的回收率在80-99%之间,相对标准偏差(RSD)为2.80-4.32%。揭示了原料中三聚氰胺残留量与成型品的三聚氰胺迁移量的正相关关系。结果表明,该法简便、快速,可准确测定食品接触材料中三聚氰胺残留量。     

HPLC-MS/MS法测定食品接触材料中6种邻苯二甲酸酯的含量

建立了测定食品接触材料中6种邻苯二甲酸酯的含量的高效液相色谱-串联质谱法(HPLC-MS/MS)。实验以Agilent ZORBAX SB-C18色谱柱为分析柱,以甲醇-0.1%的甲酸水为流动相,采用梯度模式洗脱。质谱离子源的工作模式为正离子电离模式(ESI+),流速为0.35 mL/min,采用多反应监测离子模式(MRM)进行检测定量。实验样品前处理采用了加速溶剂萃取法,明显提高了食品接触材料中邻苯二甲酸酯的提取效率。结果表明:6种邻苯二甲酸酯在其线性范围内线性关系良好(R2>0.999),DPRP和BBP的定量限为1.0 ng/mL,DCHP,DNHP,DHP,DBEP的定量限为0.2 ng/mL,DPRP和BBP的检测限为0.2 ng/mL,DCHP,DNHP,DHP,DBEP的检测限为0.05 ng/mL。该方法的加标回收率为89.2%～107.5%,相对标准偏差均小于5.0%。实验表明,所建立的方法简单、灵敏度高,适用于食品接触材料中的6种邻苯二甲酸酯类增塑剂的分析检测。     

Determination of Four Types of Hazardous Chemicals in Food Contact Materials by UHPLC‐MS/MS

A simple ultrahigh‐performance liquid chromatography (UHPLC) tandem mass spectrometric method for the identification and quantification of two photoinitiators 4‐methylbenzophenone and 2‐ethylhexyl‐4‐dimethylaminobenzoate; nine plasticizers including di(2‐ethylhexyl) adipate and diisobutyl adipate; three primary aromatic amines 4‐aminobiphenyl, 4‐amino‐2′,3‐dimethylazobenzene and bis‐(4‐aminophenyl) methane and six bisphenols bisphenol F diglycidyl ether, bisphenol A diglycidyl ether, bisphenol A (BPA), bisphenol B (BPB), bisphenol E (BPE) and bisphenol F (BPF) in food contact materials has been developed. The chromatographic conditions, pre‐treatment methods and matrix effects were studied and optimized. For the determination of the four bisphenols, BPA, BPB, BPE and BPF, the UHPLC method employed a mobile phase of aqueous ammonia and methanol in binary gradient mode, and measurement was based on a triple quadrupole mass spectrometer equipped with an electrospray ionization (ESI) source operating in negative ion mode. The remaining chemicals were determined using the ESI source in positive ion mode and using the [M + NH₄]⁺ or [M + H]⁺ adducts as precursor ions for tandem mass spectrometry. The calibration graphs were linear with correlation coefficients of above 0.995. Detection limits for the method were in the range of 1–16 µg/kg. Analyte recovery values were in the range of 70–114%, and relative standard deviations were 1–14%. Under optimized conditions, the chromatographic separation was performed in 12 min. The validation data indicated that the method was effective for the determination of the four classes of hazardous chemicals in plastic packaging materials or in can lacquers. The optimized method was successfully applied to trace analysis of commercially available food contact materials. Copyright © 2014 John Wiley & Sons, Ltd.     

食品接触材料及制品1,4-丁二醇迁移量测定方法

目的建立测定1,4-丁二醇的气相色谱检测方法,确认食品接触材料及制品中1,4-丁二醇迁移量是否满足国标限量要求。方法对可降解塑料产品进行迁移试验,采用气相色谱法对迁移液中1,4-丁二醇进行分离、定性和定量检测。结果该法对1,4-丁二醇迁移量的方法检出限为0.4 mg/kg,1,4-丁二醇的含量为0~10 mg/kg时,与色谱峰面积具有良好的线性关系,相关系数大于0.995,样品加标回收率为95.2%~108.7%,测定结果的相对标准偏差为5.9%~9.7%(n=10)。结论该方法适用于食品接触材料及制品1,4-丁二醇迁移量的检测。     

Determination of Selected Perfluorinated Acids (PFCAs) and Perfluorinated Sulfonates (PFASs) in Food Contact Materials Using LC‐MS/MS

Perfluorinated compounds, including perfluorinated acids and perfluorinated sulfonates, are environmentally persistent. These compounds are commonly used in consumer products as stain/water/grease repellents in carpets and clothing, in cooking utensils as nonstick coating and in food contact materials as a coating. This paper explores the potential application of liquid chromatography coupled with tandem mass spectrometry (LC‐MS/MS) system for the measurement of selected perfluorinated acids and perfluorinated sulfonates in three different brands (A, B and C) of food contact materials, including wrapping papers, breakfast bags, baking papers and roasting bags. In this study, the highest contents of selected perfluorinated acids were identified for the breakfast bag samples (2.54–6.60 pg/cm²), especially for B and C brands with the concentration of 6.60 and 5.35 pg/cm², respectively, while the lowest content was noted in roasting bag samples (0.27–0.40 pg/cm²). The contents of perfluorinated sulfonates were inversed as compared with those of perfluorinated acids. The highest contents of selected perfluorinated sulfonates were found in roasting bag samples (1.38–5.17 pg/cm²), especially for B brand. The analysed perfluorinated sulfonates were not detected in any of the breakfast bag samples. The highest content of perfluorinated compounds were reported for B brand food contact materials. The data indicate a risk of food contamination by perfluorinated compounds from the commonly used food contact materials. Copyright © 2015 John Wiley & Sons, Ltd.     

加速溶剂萃取-GC-MS/MS法测定食品接触材料中双酚A、双酚F及其衍生物的残留量

建立了加速溶剂萃取-气相相色谱-串联质谱法测定食品接触材料(婴儿奶瓶)中双酚A、双酚F及其衍生物残留量的分析方法。样品用二氯甲烷作提取剂,用加速溶剂萃取仪进行了提取,经乙酸酐衍生化,用气相色谱-串联质谱仪进行了定性、定量分析。结果表明:BPA,BPF,BADGE,BFDG 4种化合物的回收率范围在78.9%～101.1%之间,相对标准偏差小于10%,线性关系良好,方法的检出限分别为0.2,0.1,5,5 ng/g,该方法简便、快速、灵敏度高、重复性好。     

ICP-AES同时测定废氰化镀金溶液中Au，Cu，Ni，Fe含量

为了快速测定废氰化镀金溶液中Au，Cu，Ni，Fe四种元素含量，采用一步消解直接进行ICP-AES测定。并对分析谱线、元素干扰和等离子体参数进行了讨论。结果表明，方法检出限为0．014—0．019μg／ml，加标回收率在97．3—101．0%之间，相对标准偏差（RSD）小于2．54％。该方法准确、快速、简便。应用于废氰化镀金溶液的回收生产，结果令人满意。