电感耦合等离子体—质谱法测定番茄酱中多种重金属元素的研究
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摘要
我国是目前世界第一大番茄制品出口国,加工能力位居世界第一,2009年新疆番茄酱产量达到101.83万吨,出口检验84.71万吨,货值7.39亿美元。番茄产业在新疆农业经济中占有举足轻重的地位。
     铅、镉、汞、砷、锡、铜等重金属元素一直是出口番茄酱食品安全检测项目。由于受季节生产和市场竞争的制约,出口番茄酱的检验呈现检验时间集中、检验批量大的特点,成为出口番茄酱检验的瓶颈。本文建立了番茄酱中重金属元素电感耦合等离子体-质谱检测方法,实现了一次制样,同时测定13种食品安全相关元素含量。本方法分析速度快、操作简单,方法检出限、精密度和线性范围均能满足我国及国际食品卫生标准重金属元素检测的要求。本文的主要研究内容如下:
     (1)建立了番茄酱样品的前处理方法。试验对比了电热板消解法、常压消解仪消解法和微波高压消解法;确定了微波高压消解条件;选择的消解体系是5mL硝酸+1mL过氧化氢。试验使用浊度测定法定量判断样品的消解程度,为建立最佳消解程序提供技术依据。
     (2)依照质谱分析选择核素的原则,经过同质异位素干扰分析、加合物干扰分析后,确定了13种待测元素的核素。根据待测核素的质量范围以及新疆19个地区番茄酱中稀土元素含量的调查结果,选定了可用于校止基体效应的内标稀土核素,即72Ge、115In和209Bi混合内标溶液。
     (3)试验优化了电感耦合等离子体-质谱仪的工作条件,对仪器的射频功率、雾化器流速、反应气/碰撞气流量、动能歧视的调节等20多项参数行了优化,使仪器的灵敏度及分辨率等均达到最佳测试状态。检测、评价了工作气源、纯水、试剂及样品消化体系等环节带来的重金属污染的种类和污染水平,为电感耦合等离子体-质谱检测方法的试剂空白和样品空白的控制提供了依据。试验对比了水、硝酸溶液、金溶液消除测汞时出现的严重记忆效应。
     (4)本试验对比了电感耦合等离子体-质谱仪的两种不同测定模式(标准模式与反应/碰撞池技术模式)对同一番茄酱样品的测定结果,并对数据进行统计学t检验处理,得出在测定核素52Cr、57Fe、78Se、118Sn时,两种模式测定结果存在显著性差异,从而得出电感耦合等离子体-质谱检测方法测定番茄酱样品时,可能存在由加合物离子导致的质谱干扰。本试验还对反应/碰撞池模式消除加合物离子干扰的效果进行了评价。
     (5)通过对新疆地区三年生产的番茄酱中8种重金属元素含量的统计及国家食品卫生标准的查阅,评价了本方法的标准曲线线性范围、仪器检出限和方法检出限,得出的结果满足出口番茄酱中重金属元素的检测要求。
     (6)通过对番茄酱样品中进行标准添加试验,得出各元素的添加回收率在83.8%~112.5%之间,精密度指标RSD值为0.3%~5.0%。
     (7)进行了方法验证试验,通过测定相似样品基体的标准参考物质——番茄叶,得出其测定结果与证书给定的参考值相符。
China is the largest exporter of tomato products and processing capacity is the first in the world. The tomato paste yield of Xinjiang region had reached 1,018,300 tons, export inspection was 847,100 tons in 2009, which volued at$739,000,000. Tomatoes industry occupies a pivotal position in the agricultural economy in Xinjiang.
     Lead, cadmium, mercury, arsenic, tin, copper and other heavy metals have been food safety inspection item for tomato paste export. Because of seasonal production and constraints of market competition, the inspection of tomato paste for export has some characters that is test time to concentrated and test batch for large, so it's became the choke point of tomato paste inspection for export. Testing heavy metals in tomato paste by inductively coupled plasma-mass spectrometry was built in the article, it has achieved only once sample preparation and determination of 13 elements interrelated with food safety at the same time. The method was fast and simple, the limits of detection, precision and linear range all can suffice inspection require in food sanitation standard of China and international standard.
     The main contents of the paper as follow:
     (1)Pretreatment method of tomato paste sample was established. The methods by electric-hot plate digestion, atmospheric pressure digestion and microwave high pressure digestion were contrasted by experiment, and the parameters of microwave high pressure digestion was determined; the component of digestion reagent is 5mL nitric+1mL hydrogen peroxide. Turbidity determination was used for test solution of digestion, it could provide technical basis for the best digestion procedure establishment.
     (2) In accordance with the principles of selected nuclides in mass spectrometry, nuclides of 13 kinds of elements were identified by isobaric interference analysis and adduct interference analysis. According to mass range of the analyzed nuclides and investigate results of 19 regions in Xinjiang, internal standard rare earths elements for regulating matrix effect were selected, they are 72Ge,115In and 209Bi. These nuclides make up mixed internal standard solution.
     (3) Working conditions of ICP-MS instrument were optimized; include RF power, nebulizer flow rate, reaction gas/collision gas flow rate, kinetic energy discrimination and other more than 20 parameters, so that the sensitivity and resolution of instrument attained the best test condition. The pollution elements from gas supply, water, reagent, sample digestion reagent and other aspects were analyzed and evaluated, it provided a basic data for control of reagent blank and sample blank. The effect of eliminating Hg memory interference had been evaluated by test of the water, nitric acid solution and aurum solution.
     (4) The results of two different ICP-MS determination mode (standard mode and reaction/collision cell mode) on the same tomato paste sample were compared in this study, and the data was treated by T test of statistics. The statistic results showed that two determination modes exist distinct difference when 52Cr, 57Fe,78Se and 118Sn were analyzed, it indicate the method may exists mass interference from adduct ions. The study evaluated also on the effect of eliminating adducts ion interference through different ways.
     (5) According to 8 heavy metals content of tomato paste in three years in Xinjiang region and national food hygiene standards, the method linear range, the limits of detection for instrument and the limits of detection for method had been confirmed. All test results satisfy requirements of determination for tomato paste export.
     (6) Through standard addition experiments to sample, the results showed that recoveries of all elements are 83.8%~112.5%, precision RSD are 0.3%~5.0%.
     (7)The results of method verification test showed the test results accord with the value of reference standard certificate entirely. The standard reference material which was made of tomato leaves have similar sample matrix with tomato paste.
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