冻干松茸粉中总砷及无机砷的含量测定

目的测定冻干松茸粉中总砷及无机砷的含量。方法采用电感耦合等离子体质谱法(inductively coupled plasma mass spectrometry,ICP-MS)、原子荧光光谱法(atomic fluorescence spectrometry,AFS)、液相色谱-电感耦合等离子体质谱法(liquid chromatography with inductively coupled plasma mass spectrometry,LC-ICP/MS)3种方法分别测定松茸中总砷及无机砷含量。结果ICP-MS、AFS测定冻干松茸粉中总砷含量分别为71.7、0.556 mg/kg,LC-ICP/MS测定冻干松茸粉中无机砷含量为0.0114 mg/kg。结论冻干松茸粉中砷主要以有机态存在,且不同检测方法以及前处理方式都会对实验结果产生影响。     

食品中硒的有机形态分析研究进展

硒是人体必不可少的微量元素, 不同形态的硒对人体的功能不同, 其中有机硒在抗氧化、抗癌、抗病毒、提高免疫力等方面对人体有重要作用。人体获取硒的途径主要通过膳食摄取, 如食用天然富硒食品、人工合成有机硒产品及有机硒强化剂等。市场上的富硒食品质量参差不齐, 为合理地评价食品中硒的摄入形态和水平, 对食品中硒的形态及含量的检测是近年来研究的一个重点。本文对食品中有机硒检测分离、形态分析以及含量测定等进行了综述, 并对以液相萃取法和酶解法为主的分离方法, 以气相色谱-电感耦合等离子体质谱法(gas chromatography-inductively coupled plasma spectrometry, GC-ICP-MS)、高效液相色谱-电感耦合等离子体质谱法(high performance liquid chromatography-inductively coupled plasma spectrometry, HPLC-ICP-MS)、高效液相色谱-串联三重四级杆质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)以及电泳-电感耦合等离子体质谱法(capillary electrophoresis-inductively coupled plasma spectrometry, CE-ICP-MS)为主的检测方法等研究进展进行了总结, 以期对食品中有机硒的检测提供相应的理论依据, 促进食品中有机硒检测标准的发展。     

ICP-MS和ICP-OES法检测粉条中铝含量的比较研究

为确定粉条中铝元素含量检测最适用的方法,将3批次粉条样品进行微波消解法处理,消解液分别使用电感耦合等离子体质谱法(inductively coupled plasma mass spectrometry,ICP-MS)和电感耦合等离子体发射光谱法(inductively coupled plasma optical e...     

氢化物发生-电感耦合等离子体串联质谱法分析大米中的无机砷

建立氢化物发生-电感耦合等离子体串联质谱(inductively coupled plasma-tandem mass spectrometry,ICP-MS/MS)法直接测定大米中无机砷含量的高通量分析方法.采用硝酸-双氧水提取大米样品中的无机砷,以5 mol/L盐酸作为预还原剂将砷(V)还原为砷(III),在多模式...     

超级微波消解-串联四极杆电感耦合等离子体质谱法测定当归中27种无机元素

目的 建立超级微波消解-串联四极杆电感耦合等离子体质谱法(tandem quadrupole inductively coupled plasma mass spectrometry, ICP-MS/MS)测定当归中27种无机元素含量的分析方法。方法 以当归为材料, 通过优化消解酸体系与超级消解平台工作参数进行试样消解, 在线引入500 μg/L混合内标以校正信号漂移。在等离子气流速为15.0 L/min、辅助气流速为0.9 L/min、功率为1550 W时, 采用ICP-MS/MS测定试样中27种无机元素的含量。结果 所测27种元素线性关系良好, 相关系数在0.9993~1.0000之间, 检出限为0.00003~0.13548 mg/kg, 定量限为0.00010~0.40643 mg/kg, 回收率为93.90%~115.40%, 精密度在0.02%~2.55%之间; 国家标准物质-黄芪的测定结果均在推荐值范围以内。结论 该方法操作简单、灵敏度高, 适用于当归中27种无机元素含量的测定。     

高效液相色谱-电感耦合等离子体-串联质谱测定水产品中5种形态砷

建立高效液相色谱-电感耦合等离子体-串联质谱法（high performance liquid chromatography-inductively coupled plasma tandem mass spectrometry,HPLC-ICP-MS/MS）测定水产品中5 种形态砷的检测方法。利用MS/MS模式,以质量转移的方式消除干扰,流动相由10 mmol/L C2H3NaO2、3 mmol/L KNO3、12 mmol/L NaH2PO4等组成,采用梯度洗脱,As7阴离子交换色谱柱分离。结果表明：5 种形态砷可完全分离,三价砷、二甲基砷、一甲基砷、五价砷和砷甜菜碱都具有良好的线性相关系数,检出限依次为0.005 94、0.005 28、0.008 17、0.008 41、0.011 70 mg/kg,满足检测要求;加标回收率为83%～116%,相对标准偏差均小于5%;该方法具有简便快捷、准确度高、分离明显、检测效率高等特点,可对水产品中多种形态砷进行评价分析。     

电感耦合等离子质谱法同时测定昆明市售乳扇和乳饼中12种元素

建立电感耦合等离子体质谱法(inductively coupled plasma mass spectrometry,ICP-MS)同时测定昆明市售乳扇、乳饼中12种元素的含量.以浓硝酸为消解液,经石墨消解仪前处理后,采用ICP-MS同时检测12种元素,内标法定量.12种元素在0～100μg/L浓度范围内有较好的线性关...     

电感耦合等离子体质谱联用技术在食品中5种元素形态分析中的应用

电感耦合等离子体质谱法(inductively coupled plasma mass spectrometry, ICP-MS)在微量元素分析, 尤其是元素形态分析中起着越来越重要的作用。随着对食品中元素存在形态的含量的要求越来越多, ICP-MS单机技术已经不能满足现有的检测需求, ICP-MS联用技术逐渐发展起来。ICP-MS联用技术主要采用色谱进行分离, 电感耦合等离子体质谱法进行检测, 主要的联用技术有液相色谱、气相色谱、毛细管电泳等与电感耦合等离子体质谱仪联用。铅(Pb)、砷(As)、汞(Hg)、锡(Sn)等元素在自然界中的存在形态很多, 其存在形态不同, 毒性相差也比较大; 而硒(Se)作为人体必需的微量元素, 硒的存在形态决定了人体对硒的吸收, 间接影响了硒在人体的生物学活性。本文主要对电感耦合等离子体质谱法联用技术在分析食品中存在的5种微量元素Pb、As、Hg、Sn、Se的应用研究进展进行了概述, 以期为深入研究食品重金属元素的形态标准提供参考。     

超级微波消解-电感耦合等离子体质谱/发射光谱法测定再生聚对苯二甲酸乙二醇酯瓶片中31种元素含量

目的 建立超级微波消解-电感耦合等离子体质谱/发射光谱法测定再生聚对苯二甲酸乙二醇酯(recycled polyethylene terephthalate, rPET)瓶片中锑(Sb)、铬(Cr)、锌(Zn)等31种元素含量的筛查分析方法。方法 采用超级微波对瓶片样品进行消解,采用电感耦合等离子体发射光谱法(inductively coupled plasma optical emission spectrometry,ICP-OES)和电感耦合等离子体质谱法(inductively coupled plasma mass spectrometry,ICP-MS)分别测定7种和24种元素含量,并用建立的方法对从工厂收集的40批次rPET瓶片样品进行检测。结果 方法检出限为0.02～5.24mg/kg,相关系数高于0.997,加标回收率为76%～118%,其相对标准偏差(relative standard deviations, RSDs)为0.7%～9.4%。40批次r PET样品都检出了Sb元素,含量范围为126～208 mg/kg。有少量样品有Cr元素或Zn元素检出。结论 该方法...     

电感耦合等离子体质谱法同时检测贵州省芸豆中13种元素含量

目的 建立电感耦合等离子体质谱法(inductively coupled plasma mass spectrometry,ICP-MS)同时测定贵州芸豆主产地28份芸豆样品中Na、Mg、P、Ca、Cr、Mn、Fe、Cu、Zn、As、Cd、Hg、Pb 13种元素的定量分析方法.方法 采用主成分分析和聚类分析方法分析贵州...     

Lead, chromium, tin, iron and cadmium in foods in welded cans

The levels of lead, chromium, tin, iron and cadmium in fruit and vegetables in welded tinplate cans were determined by atomic absorption spectrophotometry. The levels found were compared with those in foods in soldered tinplate cans and fresh foods. The results show that the lead levels in foods in welded cans were much lower than those in similar foods in soldered cans. Foods in unlacquered welded cans contain much more lead, chromium and tin than foods in lacquered welded cans. The cadmium and iron levels in canned fruit and vegetables in welded cans were similar to those found in the corresponding fresh foods.     

Effect of sterilisation and storage conditions on the migration of bisphenol A from tinplate cans of the Lebanese market

The use of bisphenol A (BPA) in lacquer coating of food cans has been restricted by different authorities in many countries, such as in Europe. However, such regulation does not exist in many other countries including Lebanon. Due to the lack of data on the quality of Lebanese can production; this study investigates the migration of BPA from two types of tinplate cans manufactured in Lebanon, before and after sterilisation. Cans were analysed under different storage conditions (time and temperature) and filled with an aqueous simulant. The determination of BPA was carried out using UPLC with fluorescence detection, and further confirmed by MS detection. After sterilisation BPA levels drastically increased from an average of 0.15 to 109 µg/kg, giving a BPA migration around 10.5 µg/dm² for both types of cans. Storage temperature and time had no significant influence on BPA levels in sterilised cans (p-value > 0.05); however, these factors significantly affected BPA levels in non-sterilised cans.     

低温下采用快速液相色谱-质谱联用法分析包装食品中UV油墨光引发剂的迁移

A fast method of liquid chromatography coupled to tandem mass spectrometry(LC-MS/MS) was developed for the analysis of eleven UV ink photoinitiators in packaged food.Chromatographic separation was achieved in a pentafluorophenylpropyl (PFPP) column at 5X2 and acetonitrile:25mM formic acid-ammonium formate(pH 2.7) in gradient elution. To reduce sample treatment,a QuEChERS(quick,easy,cheap,effective,rugged and safe) method for the extraction and clean-up of UV photoinitiators in packaged foods was evaluated.Triple quadrupole working in H-SRM on Ql mode was used for both quantitation and confirmation purposes and the most intense and selective transitions were chosen.Quality parameters of the developed QuEChERS LC-MS/MS method were established and applied for the analysis of photoinitiators in food packaged at ng/kg levels.     

Corrosion behaviour of tinplate cans in contact with tomato purée and protective (inhibiting) substances

The dissolution of iron and tin from tinplate cans filled with tomato purée (pH 4.34) and dioctyl sebacate oil (DOS), essential onion oil (EOO) or potassium nitrate was studied using atomic absorption spectroscopy (AAS), while nitrate was determined using high-performance liquid chromatography (HPLC). The maximum values found in cans were up to 284 mg kg^?1 for tin and 513 mg kg^?1 for iron at elevated storage temperature. Results indicated that the addition of EOO to tomato purée prevents the corrosion process in the case of tin, where concentrations were lowered from 223 to 28 mg kg^?1 for cans with DOS oil and EOO at 20°C, respectively (inhibition rate of 87%). On the other hand, the presence of EOO enhanced the corrosion process for iron increasing the concentration from 15 to 46 mg kg^?1 during 7 months of storage, although this value did not exceed maximum permitted value (50 mg kg^?1). In cans with tomato purée and potassium nitrate, dissolution of tin started after 30 (36°C) and 60 (20°C) days of storage as a consequence of nitrate action, which act as a corrosion accelerator. Since the addition of EOO improves the taste of canned tomato purée, its potential use as a corrosion inhibitor would be of interest.     

高效液相色谱串联质谱法测定蔬果中啶酰菌胺和环酰菌胺残留

建立蔬菜和水果中啶酰菌胺和环酰菌胺的高效液相色谱串联质谱检测方法。将试样中残留的啶酰菌胺和环酰菌胺用含1%乙酸的乙腈溶液均质提取,提取液混合使用乙二胺-N-丙基硅烷和十八烷基硅烷键合相基质分散净化,用高效液相色谱串联质谱检测和确证,外标法定量;方法通过空白基质溶液稀释标准建立校正的标准曲线,以消除基质效应。结果表明：啶酰菌胺和环酰菌胺在1～100μg/L范围内具有良好的线性关系,相关系数分别为0.9996和0.9997;在5～50μg/kg范围内,平均添加回收率在77.7%～93.8%之间,相对标准偏差在2.1%～6.3%之间。啶酰菌胺和环酰菌胺方法定量限分别为1.32μg/kg和1.20μg/kg,检出限分别为0.395μg/kg和0.361μg/kg。     

Separation and characterization of phenolic compounds in argan fruit pulp using liquid chromatography–negative electrospray ionization tandem mass spectroscopy

Liquid chromatography (LC) coupled to negative electrospray ionization (ESI) tandem mass spectrometry (MS/MS) was used for the sensitive identification of phenolic compounds in argan fruit pulp. Sixteen compounds were identified, mainly flavonoid glycosides and flavonoid aglycons.     

Migration of iron,lead, cadmium and tin from tinplate-coated cans into chickpeas

Migration studies of trace metals were carried out on coated chickpea cans marketed in Lebanon. Four elements – iron (Fe), tin (Sn), lead (Pb) and cadmium (Cd) – were analysed by atomic absorption spectrometry (AAS) after microwave digestion. Over 3 months, three different storage temperatures (5°C, room temperature and 40°C) were tested. In all cases, the migration of Fe reached a plateau after around 50 days of storage, while the migration of Pb was slow till 50 days, then it increased rapidly. Cd and Sn levels did not increase. Moreover, no effect of temperature was observed in the case of Fe, whereas Pb levels showed slower migration in cans stored at 5°C. Comparing cans from different chickpea brands (Lebanese and foreign) showed that the characteristics of the container have an effect on metal release.     

Determination of the change of flavonoid components as the defence materials of Citrus unshiu Marc. fruit peel against Penicillium digitatum by liquid chromatography coupled with tandem mass spectrometry

A healthy fruit peel of Citrus unshiu Marc. and one infected by Penicillium digitatum were analysed for flavonoids via high-performance liquid chromatography coupled with tandem mass spectrometry (HPLC–MS/MS) in the positive mode with selected ion monitoring (SIM). Among 16 flavonoid components characterised in C. unshiu Marc., four flavanones and nine flavones were identified for the first time. The identified compounds were quantified by HPLC–UV. To investigate the function of the flavonoids as defence materials, the flavonoid content change of the fruit peel inoculated with P. digitatum was monitored by HPLC. The flavonoid concentration in the infected fruit peel decreased initially after the infection and then gradually increased before finally progressively decreasing.     

High Vacuum Flame Sterilized Fruits: Influence of Can Type on Storage Stability of Vacuum Packed Peach and Pear Slices

The feasibility of using enameled tin and tin-free steel (TFS) cans for processing oxygen sensitive fruits by high vacuum flame sterilization was evaluated. Through 18 months storage at ambient temperatures, the appearance and quality of the HVFS peaches and pears remained acceptable for all can types. Fruits packed into plain tin cans appeared brighter and tasted tangier than those packed into TFS or inside-enameled tin cans. Texture, pH and titratable acidity of fruit were not measurably affected by variation in can types. Mechanical deaeration followed by flame sterilization, produced a product with quality comparable to that achieved in flame deaerated packs.     

Lead content in grapefruit juice and its uptake upon storage in open containers

The lead contents of 52 samples of grapefruit juice, 14 packaged in glass, eight in waxed paperboard, and 30 in tin-coated carbon steel containers, were determined. Only those juices packaged in metal cans contained measurable amounts of lead, (< 1–27 μg litre-¹) averaging 7-7 μg litre-¹. Leaching studies were carried out on juices stored, under refrigeration, in opened containers for up to 30 days. The lead content increased considerably with time in juices stored in tin-coated cans. For example, after 6 days of storage the lead contents of these juices ranged from 3 to 90 μg litre-¹, and averaged 30 μg litre-¹. The lead content did not increase in juices that were stored in glass, paperboard or polyethylene containers. The source of lead in the cans was traced to lead impurities in the tin coating. Higher lead impurities in the tin coating produced higher lead contents in the juice. The implications of these findings are discussed.