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1.
原子荧光法测定小麦中铅含量的研究   总被引:2,自引:1,他引:2       下载免费PDF全文
为了选择一种简便快速测定小麦铅含量的实验方法,选用小偃22、陕150、陕160、陕225和N9628等小麦品种(系)为试验材料,分别以HNO_3-H_2O_2、HNO_3-HClO_4、HNO_3-H_2SO_4为氧化剂,密封式压力罐消解小麦样品,氢化物发生—原子荧光光度计测定小麦中的铅含量。考察了小麦样品消解过程中采用混合酸的种类及用量、试样用量、还原剂硼氢化钠浓度等因素对测定结果的影响。结果发现该方法的最佳实验条件为:HNO_3-H_2O_2作为氧化剂有利于消解试样,试样用量为0.5~1g,NaBH_4浓度为2%。用此方法对实际小麦样品的回收率及方法的精度进行测定,回收率在89.8%~103.4%之间,相对标准偏差为1.90%,在0~200 ng·ml~(-1)范围内呈良好的线性关系(r=0.9997),方法的检测下限为0.02 ng·ml~(-1),可满足实际样品测定的要求。  相似文献   

2.
采用氢化物发生原子荧光法测定海南白沙绿茶和红茶中的硒含量,研究了仪器条件和还原剂等对硒原子荧光强度的影响。结果表明,最佳仪器条件为光电倍增管负高压300 V,灯电流80 mA;还原剂浓度为1.5%,载流盐酸浓度5%。该方法线性范围0~10 μg/L时,与荧光值线性关系好,回归方程为y=75.949x-8.795 4,相关系数r=0.999 8。方法检出限是0.024 μg/kg,测定标准物质中硒的回收率为97.7%~109.6%。以国家标准物质茶叶(GBW10016)为监控样品,标准物质茶叶测定值与标准值吻合。白沙绿茶和红茶硒元素含量分别是34.4和20.1 μg/kg。该方法线性范围宽、灵敏度高、检出限低,可用于茶叶等样品中硒元素含量的准确测定。  相似文献   

3.
采用微波消解方法处理剑麻叶片样品,以铟(115In)为内标元素进行校正,优化ICP-MS仪器工作参数等技术,测定剑麻叶片中微量元素钼的含量。结果表明:钼的检出限为0.025 μg/L,回收率为96%~104%,相对标准偏差(RSD)为0.87%,同时测定国家标准物质菠菜(GBW10015)中的钼,分析结果在标准值范围内,显示微波消解-ICP-MS方法具有检出限低、快速、简便、准确等特点。  相似文献   

4.
刘慧 《茶叶学报》2019,60(4):151-155
本试验分别采用干法灰化法、湿法消解法、微波消解法3种不同的消化方法作为前处理方式,用电感耦合等离子体质谱法(ICP-MS)测定红茶中15种金属元素。试验结果表明:干法灰化法处理测定的金属元素含量高于湿法消解法,而微波消解法处理测定的含量高于干法消解法。采用内标法,对各个元素的检出限、线性范围、3种前处理基本参数进行了研究,并进行了标准物质测定和精密度试验。选用微波消解法处理样品,标准物质测定值更接近标准参考值,相对标准偏差<2%,干灰化法优于湿法消解法,相对标准偏差分别为2%~3%、3%~5%。微波消解前处理方式明显优于其他两种前处理方法,简便、快速、准确率高,适用于多种金属元素的同时测定。  相似文献   

5.
茶园土壤中铅锌等元素同时多检出测定方法研究   总被引:2,自引:0,他引:2  
分别用三酸敞开式电热板消解、四酸敞开式电热板消解、二酸微波消解及三酸微波消解法对茶园土壤进行前处理,然后以电感耦合等离子体发射光谱法(ICP-OES)测定其中的铅、铜、砷、铬、镉、锌、钴含量.结果表明,四酸敞开式消解法与三酸微波消解法对土壤进行前处理,都能使土壤样品中的7种重金属元素完全消解,测定效果较理想.但三酸微波消解法因测定用时短、成本低而显得更优越.用ICP-OES法测定三酸微波消解前处理的土壤标准样品中的重金属元素时,7种重金属元素的相对标准偏差在0.03%~7.24%之间,其测定值与推荐值完全一致.对普通红壤土与铅锌矿土的加标回收结果,普通红壤土的回收率在84.0%~110.0%之间,铅锌矿土的加标回收率在94.0%~114.0%之间.方法简便、准确,而且劳动强度小,能缩短检测周期,提高工作效率.  相似文献   

6.
采用硝酸-盐酸-氢氟酸作消解体系,以微波消解的方法处理土壤样品,利用ICP-MS同时测定土壤样品中的4种重金属元素(铅、铜、铬、镉)。设定了最佳的样品前处理条件和仪器测定条件,在进行质谱测定时,采用In、Bi、Ge元素作为校正基体效应与信号漂移的内标元素。依据国家标准参考物质并通过加标回收试验,对方法进行了验证。结果表明:该方法所得重金属元素铅、铜、铬、镉的检出限分别为0.010、0.020、0.050、0.005μg/L,加标回收率分别为98%~106%、97%~112%、94%~118%和98%~104%;测定不同土壤标准物质,铅、铜、铬、镉测定结果均在标准值允差范围内,相对标准偏差(RSD)介于0.5%~2.5%。说明该方法稳定性好、精密度高、操作简便、成本低,适用于大量土壤样品4种重金属元素(铅、铜、铬、镉)的同时测定。  相似文献   

7.
陈韵  任安祥  李双婷 《大豆科学》2007,26(5):784-786
应用编程全自动微波消化技术处理检测样品,样品和试剂用量少,空白值低,少污染,样品消化完全,操作便捷,是一项全新的样品前处理技术.通过筛选消化试剂的种类,优化消化仪编程和原子荧光仪器检测参数测定大豆中硒的含量,灵敏度高,重现性好,加标回收率为86.4%~107.6%.  相似文献   

8.
小麦强化营养粉中钙、锌含量的盐酸浸提快速测定   总被引:1,自引:0,他引:1  
为了研究盐酸浸提快速法在测定小麦强化营养粉钙、锌含量中的应用,以5份小麦强化营养粉和小麦标准物质(GBE08503b)为材料,分别用盐酸浸提快速法和高温灰化法对样品进行前处理,再用火焰原子吸收法测定钙、锌含量.结果表明,盐酸浸提快速法的钙、锌检出限分别为0.52、0.08 μg/mL;方法精密度(RSD)分别为3.4%、2.8%,与国家标准推荐的高温灰化法相比较差异均不显著.两种方法下小麦标准物质钙、锌含量的测定值与标准值的差异性以及两种方法测定值间的差异性t检验均不显著,表明盐酸浸提快速法有较高的准确度.5份小麦强化营养粉的钙、锌质量分数用盐酸浸提法的测定值略低于高温灰化法,t检验差异不显著.试验表明,该方法快速、操作简单,适合测定小麦强化营养粉中钙、锌的含量.  相似文献   

9.
目前测定茶叶中镉所使用的预处理手段存在着操作繁琐、干法损失元素和湿法易蹦溅等缺陷,同时处理的样品少和过程不易控制,回收率偏低[1]。应用程序控制温度-湿法消解-原子吸收法测定水果蔬菜中汞的方法已有报道[2],应用该法测定茶叶中镉的文献在国内外尚未见到。我们对此进行的试验得到:回收率85.5%~113.6%,相对标准偏差<5%。结果与标准物质相对照,经t检验无显著差异。1 试验条件1.1 仪器与试剂1.1.1 仪器ADE-V型自控电热消解器(核工业北京化冶院);Spectr AA·880型石墨炉检测器原子吸收分光光度计,附PSD (美国Varian公司);…  相似文献   

10.
《中国茶叶》2008,(3):37-37
采用微波和高压密封罐分别消解茶叶及相应地域的土壤样品,以电感耦合等离子体质谱法测定不同地域茶叶及土壤样品中的稀土元素含量。方法的检出限在0.04-0.07ng/g之间,对标准样品6次测定值的相对标准偏差为1.78%~5.84%,相对误差小于10%。  相似文献   

11.
氢化物发生-原子荧光法测定大豆色拉油中的痕量砷   总被引:7,自引:0,他引:7  
陈国友 《大豆科学》2003,22(1):69-72
研究利用干灰化法消解大豆色拉油 ,用氢化物发生 -原子荧光法测定其中的痕量砷 ,对消化方法、样液介质及酸度、还原剂 (KBH4)浓度、干扰离子、还原掩蔽剂等影响因素进行了探讨、得出试验的最佳条件。试验结果准确 ,灵敏度高 ,重现性好 ,方法简便、快速 ,适合于植物油中痕量砷的测定 ,方法的回收率在 86 .9%~ 98.0 %之间 ;线性范围为 0~ 2 0 0ng ml;检出限为 0 .19ng ml。  相似文献   

12.
Ash content is an important quality control parameter in milling industry. Measurement of ash content is routinely performed using standard ash analysis method in which the sample is burned at 500–600 °C for 5–6 h. However, this method is not convenient for industrial applications, and thus, rapid and reliable methods are needed to be developed. The aim of this study was to develop a new method for ash analysis to be used in wheat milling fractions by using laser induced breakdown spectroscopy (LIBS). LIBS is an optic based multi-elemental, spectroscopic method which can analyze high number of samples in a considerably short time. In the study, wheat flour, whole wheat meal and semolina samples with different ash contents were analyzed using LIBS, and the spectra were evaluated with partial least squares (PLS) method. The results were correlated with the ones taken from standard ash analysis method. Calibration graph showed good linearity with the ash content between 0.48 and 2.44%, and 0.997 coefficient of determination (R2). Limit of detection for ash analysis was calculated as 0.11%. The results indicated that LIBS is a promising and reliable method with high sensitivity for routine ash analysis in milling industry.  相似文献   

13.
研究建立了普洱茶中9种金属元素含量的测定方法,样品经微波消解后,采用分子量相近原则选择45Sc、73Ge、115In、209Bi之一作为内标,用电感耦合等离子体质谱法(ICP-MS)同时测定普洱茶中铅、砷、镉、铬、锰、铜、锌、镍、硒的含量.检出限为0.0034~0.3100 mg/kg;在1.0~50.0 ng/mL线...  相似文献   

14.
The growing interest in β-glucans and the dietary recommendations of an exact daily intake will require rapid and accurate quantification methods of β-glucans that can be used routinely by the food industry. The objective of the present study was to adapt the standard enzymatic procedure (Megazyme method) to quantify (1-3)(1-4)-β-D-glucans to micro-plate format and further application to analyze cereal based samples with a wide range of (1-3)(1-4)-β-D-glucan content (from 0.27–75%). The samples used in this study included two breads (wheat and barley/wheat), barley flours (4% and 8% β-glucans) and two samples of oat bran (28% and 75% β-glucans). Results showed that there was no significant differences in the quantification of β-(1,3)(1,4)-D-glucans in different samples by using the Megazyme method or the micro-method. The methodology developed was also compared in terms of sensitivity and reproducibility with the results obtained by the Megazyme kit method and no differences were observed. In conclusion, the developed method allows the β-glucan quantification (specifically for mixed-linkage [(1-3)(1-4)]-β-D-glucan) to be conducted rapidly and by an efficient and sensitive micro-method in a wide range of concentrations.  相似文献   

15.
采用自主研制的黄曲霉毒素B1胶体金免疫定量检测卡,建立花生、玉米、大米、小麦等粮油农产品中黄曲霉毒素B1的定量分析方法,4种样品检测的线性范围为1.0~20.0μg/kg,R2>0.97,方法的定量限为1.0 μg/kg,样品加标回收率为75%~106%,RSD<20%。胶体金免疫层析法与免疫亲和柱净化-HPLC法相比,相对误差<15%,具有简便快速、灵敏度高、重现性好等特点,适用于粮油农产品及制品中黄曲霉毒素B1 筛查,样品检测时间只需15min,检测成本低于其他方法。  相似文献   

16.
小麦淀粉膨胀体积和直链淀粉含量的研究   总被引:10,自引:4,他引:10       下载免费PDF全文
为了了解陕西关中小麦品种与澳大利亚西部小数点麦品种间淀粉品质的差异,以参加陕西关中小麦品种区域试验的15个小麦品种(系)、西澳8个面条用小麦品种为材料,通过比较和相关分析的方法研究了小麦淀粉的膨胀体积、直链淀粉含量及春相互间的关系。结果表明,陕西关中和澳大利亚西部小麦品种的淀粉膨胀体积平均值分别为28.91和28.72ml/g,直链淀粉含量平均值分别为26.39%和26.14%;小偃503、小偃137和西农383表现出较高的淀粉膨胀体积(依次为31.90、31.67和29.59ml/g)和较低的直链淀粉含量(依次为20.39%、23.85%和24.25%),已达到了澳大利亚小麦品种的水平;膨胀体积与直链淀粉含量呈极显著负相关。  相似文献   

17.
In farm‐scale biogas systems, different kinds of manure are the most important substrate for anaerobic digestion, but result in low biogas yields. Biogas production can be increased by complementing the manure with forage crops, in codigestion. The aim of this study was to evaluate grass‐clover (GCS) and whole‐crop barley silages (WCB) in codigestion with manure from organic and conventional dairy production systems on biogas production, microbial community, degree of degradation and gas quality at different organic loading rates by addition of soya bean meal and wheat grain, which are rich in protein and starch. Four continuous stirred anaerobic laboratory‐scale reactors were used, and the codigestion resulted in additive effects on biogas production, but no synergistic effects. The highest biogas yield was obtained in reactors receiving WCB independently of manure types, for both experiments (7,416 ml/day and 10,978 ml/day respectively). The degradation efficiency, measured as the reduction in volatile solids was, on average, six percentage units higher in the reactors receiving manure from conventional compared with organic dairy cows, probably because of a higher concentration of undigested fibre and proteins in conventional cow manure. Microbiological analysis by illumina sequencing illustrated low impact of both manure types on the reactor community and only small differences between the reactors receiving GCS and WCB. However, addition of soya bean meal and wheat grain changed the community in all reactors. The ratio between Firmicutes and Bacteroidetes was comparably higher in reactors having the highest gas production and methane yield.  相似文献   

18.
为了解洛阳市小麦籽粒元素富集特征基于土壤元素含量的关系,对洛阳市土壤硒高背景区种植的小麦和土壤进行了系统采集,测定了土壤25项全量指标、6种元素的有效态指标、7种元素的形态指标及小麦籽粒12种微量元素含量,分析了土壤和小麦籽粒中有益元素和重金属元素的含量特征、富集规律以及小麦籽粒微量元素与土壤元素的相关性。结果表明,研究区土壤富集硒和钼,小麦籽粒中钼、锌、硒、铜的富集系数均大于15%,富硒小麦的比例为69.11%,籽粒镉、砷、铅、汞、铬含量均低于全国平均值。小麦籽粒中硒、钼、砷含量与土壤pH值均呈显著正相关,镉、铬、镍含量与土壤pH值均呈显著负相关,锗含量与土壤pH值呈正相关,铜、锌含量与土壤pH值呈负相关,汞、铅、氟含量与土壤pH值均无相关性。研究区小麦籽粒具有有益元素丰富、有害元素含量低的特征,因而该地区是富硒富钼同时锌铜丰富的特色小麦有利地区。  相似文献   

19.
The development of anin vitroenzymic batch method for pretreatment of cereal samples prior toin vitrofermentation is presented. A statistical experimental design is described and the importance of bile and pepsin for the digestibility of starch was investigated. Day-to-day variation was studied by measuring glucose released and total starch in the digestion residue of rye flour. Four samples, wholemeal rye flour and bread, wholemeal and white wheat breads, were tested to evaluate the performance of the digestion procedure. Pepsin and bile enhanced the hydrolysis of slowly digestible starch. The extent of starch hydrolysis in rye and wheat breads (93–95%) was reproducible and about the same as using thermostablealpha-amylase. More soluble fibres were released from the wholemeal rye bread than from the wholemeal wheat bread. The procedure is an efficient method for the removal of starch and protein under physiological conditions prior toin vitrofermentation. The method can also be used as a tool for studying the solubility of dietary fibre (DF).  相似文献   

20.
建立了奶茶中三聚氰胺的HPLC测定方法。适用检测奶茶中三聚氰胺的HPLC条件为:色谱柱SunfireC18柱(250mm×4.6mmID:5μm),流动相由0.008mol/L辛烷磺酸钠和乙腈组成,柱温30℃,流速1.0ml/min,检测波长236nm,外标法定量。分析了市场上奶茶产品的三聚氰胺含量,发现少数奶茶产品中三聚氰胺的含量超过了国家暂行限量标准的2.5mg/kg。  相似文献   

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