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1.
本实验建立了氢化物发生原子荧光光谱法测定饲料中砷的方法,并对分析条件包括介质酸度、硼氢化钾浓度和载气流速等进行优化。在优化条件下,砷的检测限为0.04 ng/mL,样品加标回收率为95.8%~99.7%,此方法可用于饲料中砷的测定。  相似文献   

2.
建立气相色谱-串联质谱法测定饲料中α-硫丹、β-硫丹、硫丹硫酸盐的方法。饲料样品经过粉碎,乙腈提取,浓缩尽干,正己烷溶解,硅藻土固相萃取柱(SPE)小柱净化。采用Agilent122-5532UIDB-5MS(30 m×0.25 mm,0.25μm),以流速1.0 mL/min高纯氦为载气,使用电子轰击离子源(EI),多反应监测模式(MRM)检测,外标法定量。结果表明,硫丹在5~1 000μg/L浓度范围内线性良好,相关系数为99.96%~99.97%。方法的检出限和定量限分别为1μg/kg和4μg/kg。4、8、20μg/kg的平均加标回收率为79.4%~100.3%,方法的相对标准偏差为5.2%~13.8%(n=5)。检测方法快速高效、检出限低、准确度和精密度高,能够满足饲料硫丹检测的需求,可用于饲料中硫丹的检测。  相似文献   

3.
高效液相色谱法测定饲料中的违禁药物氯丙嗪   总被引:6,自引:0,他引:6  
试验制定了氯丙嗪的在饲料中残留的HPLC检测方法。高效液相色谱条件为分析柱C_(18)反相色谱柱(250×4.6mm,5μm),流动相为35mmol/L NH_4Ac∶乙晴=35∶65,按0.05%的比例加入三乙胺,流速:2.0mL/min,紫外检测波长:257nm。实验表明,氯丙嗪在0.05~5.00μg/mL的范围内线性良好(r=0.99996)。经过对饲料添加0.50、1.00、2.50μg/g3个浓度,证明此提取条件的回收率在80%以上。该方法快速简便,灵敏度高。最低检测限为0.05μg/mL。  相似文献   

4.
高效液相色谱法测定饲料中替米考星含量   总被引:1,自引:0,他引:1  
本实验建立了测定饲料中替米考星含量的高效液相色谱(HPLC)检测方法。将2g饲料样品,经乙腈、乙腈-磷酸二氢钾缓冲液提取后过C18萃取柱净化、蒸干、流动相溶解后进行HPLC检测分析。流动相检测波长为290nm,流速1.0mL/min。结果表明:在1~500μg/mL的浓度范围内替米考星的峰面积(顺式和反式异构体的峰面积之和)与浓度呈良好的线性关系(r=1),平均回收率为81.4%以上,RSD小于6.1%,检测限为1μg/g。  相似文献   

5.
采用原子荧光光谱法测定饲料中总砷的含量,仪器的参数为:灯电流80mA;负高压320V;积分时间3s;泵速60r/min;主气650mL/min;辅气800mL/min。方法的线性范围为0~25ng/mL,r=0.9999,平均回收率达97.8%。与国标法试验对比,两方法相对偏差在0.5%~4.4%之间。本方法具有灵敏度高、检出限低、操作简便、省时、快捷的特点。  相似文献   

6.
采用反相高效液相色谱法(RP-HPLC)测定了硝碘酚腈含量。以乙腈-0.01 mol/L磷酸盐pH6.5(20∶80,V/V)为流动相,Agilent Zorbax SB-C18色谱柱(4.6 mm×250 mm,5μm),流速1.0 mL/min,柱温25℃,检测波长273 nm。结果表明,在0.050~1.20 mg/mL范围内硝碘酚腈浓度与峰面积呈良好线性关系(r=0.9995),最低检出浓度为2.5 ng/mL,最低定量浓度为5.0 ng/mL。低、中、高3种浓度回收率分别为100.21%、99.07%、101.90%,RSD=0.48%(n=9)。本方法专属性强,准确、简便、灵敏度高,结果稳定,可用于硝碘酚腈的含量测定。  相似文献   

7.
采用原子荧光光度法检测砷时,不需接触紫外分光光度法测定砷时所需的三氯甲烷、三乙胺等有机溶剂,可以减少对检验人员的身体伤害。此方法操作简单易行,所需检测时间短,可以较大地提高检测效率。鱼粉样品经灰化后再经盐酸消解,断续流动进样,在硼氢化钾+酸体系中,采用氢化物发生—原子荧光光谱法测定鱼粉中砷含量。线性范围:0~200ng/mL;相关系数可达到0.9997;回收率可以达到76.2%~93.4%以上,批内变异系数≤3.9%,批间变异系数≤7.5%。该方法具有较高的准确度与灵敏度,能够满足鱼粉样品中砷含量的检测要求。  相似文献   

8.
为建立气相色谱外标法测定饲料添加剂丙二醇(包膜型)的含量,本研究采用中国科学院兰州化学物理研究所色谱中心PEG-20M毛细管色谱柱(30 m×0.25 mm×0.25μm);柱温150℃,保持6 min;进样口温度270℃;检测器温度280℃;检测器为火焰离子化检测仪(Flame Ionization Detector,FID);载气为氮气(N2);色谱柱流量1.5 mL/min;进样模式为分流进样;进样1μL,分流比为20:1进行测定。结果显示丙二醇在1 mg/mL~5 mg/mL的检测浓度范围内呈良好线性关系(r2=0.999 6),最低定量限为3.2μg。该方法操作简便、灵敏、准确,适用于饲料添加剂产品中丙二醇的含量控制。  相似文献   

9.
为了能够准确地测定鸡蛋中阿莫西林的残留,本试验建立了高效液相色谱-二级管阵列检测器(HPLC-DAD)方法来检测鸡蛋中阿莫西林残留。采用乙腈沉淀蛋白提取鸡蛋液中的阿莫西林,以超纯水饱和的二氯甲烷作为进一步萃取纯化的溶剂,0.01 mol/L磷酸二氢钾溶液(pH=5.5)和乙腈溶液为流动相,流速为1.0 mL/min,检测波长为230 nm,样品进样量为20μL,柱温为30℃的色谱条件对鸡蛋中阿莫西林残留进行检测。结果显示,阿莫西林的质量浓度范围为0.05~100.00μg/mL,与峰面积具有良好的线性关系(R2=0.999 8);该方法的重复性、精密度和稳定性均良好,相对标准偏差在2.0%以内;平均加样回收率介于82.89%~89.92%,相对标准偏差介于1.68%~2.71%;阿莫西林检测限为0.025μg/mL,定量限为0.050μg/mL。结果表明,本试验所建立的HPLC-DAD方法操作过程简便、稳定性好、灵敏度高,可适用于鸡蛋中阿莫西林残留的准确检测。  相似文献   

10.
高效液相色谱法测定饲料中三聚氰胺   总被引:1,自引:0,他引:1  
采用高效液相色谱法测定饲料中三聚氰胺含量。色谱柱为Waters Xterra柱(4.6mm×150mm,5μm);流动相为乙腈:10mmol/L辛烷磺酸钠-柠檬酸缓冲液(10∶90,V∶V),检测波长为240nm,流速1.0mL/min,进样量20μL,保留时间约6.23min。三聚氰胺在1.0~50μg/mL范围内具有良好的线性关系(R2=0.99996),在添加浓度为20~100mg/kg范围内,三聚氰胺添加回收率在90%~95%,RSD小于5%。  相似文献   

11.
为完善止痢散质量标准,采用氢化物发生-原子荧光光谱法对止痢散中三氧化二砷的含量测定进行了研究。载流为3.0%盐酸溶液,还原剂为含0.5%氢氧化钾的1%硼氢化钾溶液,氩气载气流量为600mL/mL,砷空心阴极灯电流为60mA。砷元素进样浓度在0~100ng/mL范围内与荧光强度值呈良好的线性关系(r=0.9999);样品平均回收率为95.3%(n=6),RSD为1.9%。本方法简便、准确度高、重复性好,为进一步控制止痢散的质量提供了依据。  相似文献   

12.
畜禽饮用水中砷在锌和酸作用产生新生态氢。在碘化钾和氯化亚锡存在下,使五价砷还原为三价砷。三价砷与新生态氢生成砷化氢气体。通过乙酸铅棉花去除硫化氢的干扰,然后与溶于三乙醇胺-三氯甲烷中的二乙氨基二硫代甲酸银作用,生成棕红色的胶态银,比色定量。结果试样含砷量m与吸光度B呈良好的线形关系,其回归方程为m=3.884 6×B-0.215 2,相关系数r=0.999 3,检出限为0.01 mg/l,对畜禽饮用水中的砷进行测定,相对标准偏差1.3。结论:方法灵敏,结果准确,适用于畜禽饮用水中砷的快速测定。  相似文献   

13.
Levels of arsenic, cadmium, copper, mercury and lead were determined in approximately 650 samples of liver and kidney from cattle, swine and poultry slaughtered in Canada during 1979-81. In addition zinc levels were determined in livers and kidneys from swine, and selenium and zinc levels were determined in the livers and kidneys from cattle. Depending on the element several methods of atomic absorption spectroscopy were used to analyze samples including flame, hydride generation, cold vapour generation and graphite furnace atomization. Analyses were also done by plasma emission spectroscopy. Levels of arsenic over 2.0 micrograms/g were detected in 0.9% of swine livers and 0.3% of swine kidneys. Cadmium levels higher than 1.0 micrograms/g were detected in 0.3% of cattle livers, 10.8% of cattle kidneys, 1.8% of swine kidneys, 0.4% of poultry livers and 0.3% of poultry kidneys. Levels of copper over 150 micrograms/g were detected in 0.4% of cattle and swine livers. Levels of lead over 2.0 micrograms/g were detected in 1.4% of poultry livers and 1.6% of poultry kidneys. The highest level of mercury detected in all species was 0.25 micrograms/g and the highest level of selenium was 1.9 micrograms/g. Zinc levels of over 100 micrograms/g were detected in 1.7% of cattle livers, 0.2% of cattle kidneys and 5.0% of swine livers.  相似文献   

14.
Twenty-four female Beagle dogs, 7-8 months old, were assigned to 4 groups. Control, low-dosage, medium-dosage, and high-dosage groups were offered 0, 1, 2, and 4 mg of sodium arsenite per kilogram of body weight per day (mg/kg/day), respectively, in their feed (equivalent to 0.0, 33.4, 66.7, and 133.4 micrograms/g in feed). On day 59, the dosage was doubled for the rest of the experiment, which ended on day 183. In general, arsenic concentrations in tissues and body fluids reflected arsenic levels in feed. Arsenic caused a dose-related decrease in food intake. Statistically significant differences in blood, liver, and kidney arsenic were detected, in most cases, between the 2 higher dosage groups and controls. The greatest differences in arsenic concentrations between groups were present in urine and hair. Results indicate that urine and hair would be the most useful specimens for chemical analysis when attempting to confirm low-level dietary inorganic arsenic exposure or poisoning.  相似文献   

15.
Young pigs, six to ten weeks of age, from two unrelated swine operations were fed a grower ration obtained from a common commercial supplier. Following ingestion of the feed for approximately two weeks, pigs in both groups developed neurological disturbances characterized by blindness, ataxia, incoordination, muscle tremors, posterior paralysis, and quadriplegia. Vocalization described as “screaming” was also observed in several animals. Necropsy findings and tissue arsenic concentrations were consistent with a diagnosis of phenylarsonic acid poisoning. The liver and kidney contained an average arsenic content of 2.9 and 1.8 mg/kg (wet weight), respectively. The feed contained 38 mg of arsenic/kg corresponding to 133 mg roxarsone (3-nitro-4-hydroxyphenylarsonic acid)/kg. This level of roxarsone is approximately three to five times higher than the levels recommended for swine rations. The feed company had placed roxarsone in the ration at levels recommended for the less toxic arsanilic acid. It was assumed that the two organic arsenicals could be added to the rations interchangeably at the same level of formulation. The present investigation indicated that roxarsone is more toxic than arsanilic acid and the margin of safety in swine rations is low.  相似文献   

16.
依据食品安全国家标准,检测铅、砷、汞和铬的前处理方法均不统一,无法实现统一处理检测。本文建立微波消解方法对乳制品进行消解,消解后的样品可同时满足用石墨炉原子吸收光谱法检测铅、铬和用原子荧光光谱方法检测砷、汞。试验结果表明,采用微波消解法处理的样品可以同时用于铅、砷、汞和铬含量的检测,微波消解法测定乳制品中铅、砷、汞和铬的含量相对偏差小,回收率高,且得到的数据参数满意,检测数据准确,大幅度缩短了样品中铅、砷、汞和铬的检测时间。  相似文献   

17.
Responding to the challenges posed by global warming, peak oil and biofuels will require a paradigm shift in the practice of agriculture and in the role of live stock within the farming system. Farming systems should aim at maximizing plant biomass production from locally available diversified resources, processing of the biomass on farm to provide food, feed and energy and recycling of all waste materials. The approach that is the subject of this paper is that the generation of electricity can be a by-product of food/feed production. The concept is the fractionation of biomass into inedible cell wall material that can be converted to an inflammable gas by gasification, the gas in turn being the source of fuel for internal combustion engines driving electrical generators. The cell contents and related structures such as tree leaves are used as human food or animal feed. As well as providing food and feed the model is highly appropriate for decentralized small scale production of electricity in rural areas. It also offers opportunities for sequestration of carbon in the form of biochar the solid residue remaining after gasification of the biomass.  相似文献   

18.
Responding to the challenges posed by global warming, peak oil and biofuels will require a paradigm shift in the practice of agriculture and in the role of live stock within the farming system. Farming systems should aim at maximizing plant biomass production from locally available diversified resources, processing of the biomass on farm to provide food, feed and energy and recycling of all waste materials. The approach that is the subject of this paper is that the generation of electricity can be a by-product of food/feed production. The concept is the fractionation of biomass into inedible cell wall material that can be converted to an inflammable gas by gasification, the gas in turn being the source of fuel for internal combustion engines driving electrical generators. The cell contents and related structures such as tree leaves are used as human food or animal feed. As well as providing food and feed the model is highly appropriate for decentralized small scale production of electricity in rural areas. It also offers opportunities for sequestration of carbon in the form of biochar the solid residue remaining after gasification of the biomass.  相似文献   

19.
采用GB 5009.93—2017《食品安全国家标准 食品中硒的测定》第一法(氢化物原子荧光光谱法)和GB 5009.93—2017第三法(电感耦合等离子体-质谱法)研究特殊医学用途婴儿配方食品中硒检测方法的适用性。7 家实验室分别对6 种特殊医学用途婴儿配方食品(包括3 类配方)和婴儿配方乳粉质控样品中的硒进行测定,同时测定回收率。结果表明:GB 5009.93—2017第一法和第三法均适用于婴儿配方乳粉的检测,在特殊医学用途婴儿配方食品中各种配方的适用性有待进一步研究。  相似文献   

20.
为了进一步探讨黑素皮质素4受体(melanocortin-4 receptor,MC4R)基因对动物采食量和生长性能的影响,本研究利用基因重组和显微注射的方法建立了转猪MC4R基因的小鼠模型。采用PCR扩增、克隆测序的方法对每代转基因小鼠进行阳性鉴定,然后采用常规测定方法对F3代转基因阳性鼠与同期阴性对照鼠的体重和采食量进行了测定。结果显示:成功构建了转猪MC4R基因小鼠模型,阳性鼠与阴性鼠相比,体重和采食量均略有增加,但未达到显著水平(P>0.05)。据此推测体内超表达MC4R基因并不能像敲除掉该基因一样显著地改变机体性能。  相似文献   

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