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QuEChERS-气相色谱-质谱联用法检测茶叶中3种杀虫剂残留 总被引:1,自引:0,他引:1
目的建立QuEChERS-气相色谱-质谱联用法(gas chromatography-mass spectrometry,GC-MS)检测茶叶中的溴虫腈、啶虫脒和茚虫威3种杀虫剂残留的方法。方法通过对提取溶剂和净化剂的选择、基质效应等条件因素的改变,进行提取与净化方面的优化,对3种杀虫剂残留进行检测。结果 3种杀虫剂在0.05~1.00μg/mL范围内具有良好的线性关系,相关系数在0.9994~0.9999之间,检出限为0.005~0.010 mg/kg,加标回收率在89.0%~98.4%之间,相对标准偏差为2.14%~7.88%。结论建立的方法简便、准确、重现性好,可用于茶叶中溴虫腈、啶虫脒和茚虫威3种杀虫剂残留测定。 相似文献
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食醋中有机磷农药残留的测定 总被引:1,自引:0,他引:1
用气相色谱法(GC)分析测定并采用凝胶色谱净化(GPC)系统预处理,建立了食醋中有机磷残留量的检测方法。样品用乙腈提取,经凝胶渗透色谱柱净化,再经中等极性的毛细管色谱柱DB-1701P(30m×0.25mm×0.25μm)分离,气相色谱火焰光度检测器(FPD)检测。有机磷在食醋样品中的残留量检测的检出限为0.0040~0.050mg/kg。在样品中添加29种农药混合标准溶液,平均回收率为72.4%~120.8%,相对标准偏差为0.7%~14.5%(n=3),可满足食醋样品中有机磷农残的测定。 相似文献
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目的 建立QuEChERS前处理结合气相色谱-三重四极杆串联质谱联用法测定大蒜中敌百虫、霜霉威和氯氟氰菊酯共3种农药残留的分析方法.方法 将大蒜捣碎,用乙腈-醋酸(99:1,V:V)、无水硫酸镁、醋酸钠和陶瓷均质子提取,经无水硫酸镁和乙二胺-N-丙基甲硅烷(ethylenediamine-N-propylsilane,... 相似文献
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GC-MS分析法在猪肉氯霉素残留检测中的应用 总被引:3,自引:0,他引:3
建立了猪肉中残留氯霉素(CAP)的GC-MS分析方法。样品中CAP用乙酸乙酯提取,脂肪用正己烷去除,BondElut-C18柱纯化样品,BSTFA-TMCS衍生后用NCI源选择m/z为466的特征离子为目标离子,在SIM模式下进行GC-MS分析。被检测CAP质量浓度在0.08~100μg/kg内,方法的线性关系良好,相关系数为0.998。方法的最低检测限达到0.08μg/kg。用此方法对市场上销售的猪肉样品进行测定,结果显示:只有一份样品CAP残留量为(0.236±0.007)μg/kg,另4份猪肉样品中未检出CAP残留。应用本方法测定新鲜猪肉中CAP残留,基本上满足了灵敏、快速、准确可靠的分析方法要求。 相似文献
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目的:建立一种超高效液相串联三重四极杆质谱检测黄瓜中双炔酰菌胺含量的方法。方法:黄瓜试样经乙腈超声提取后,采用分散固相萃取法(QuEChERS)进行净化,超纯水稀释,用0.1%甲酸水和乙腈作为流动相进行液相色谱—串联质谱测定。采取电喷雾(ESI)离子源在正离子检测模式下,对双炔酰菌胺进行多反应监测(MRM),并使用外标法进行定量。结果:在0.01~0.50 μg/mL质量浓度范围内,双炔酰菌胺具有良好的线性关系,R2=0.999 8;在10,50,100 mg/mL 3种不同加标水平下,双炔酰菌胺回收率为 89.6%~96.0%,相对标准偏差(RSD)为0.72%~1.80%(n=6)。试验方法检出限为0.003 mg/kg;定量限为0.009 mg/kg。结论:试验方法前处理过程无需浓缩,操作简便,分析灵敏度高、稳定性好、重现性高,适用于黄瓜中双炔酰菌胺的定性与定量分析。 相似文献
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《Food additives & contaminants. Part A, Chemistry, analysis, control, exposure & risk assessment》2013,30(4):670-677
Eggs were used to study the determination and depletion of amoxicillin (AMO) residues after oral dosing hens (25.0 mg kg–1, 50.0 mg kg–1 body weight), once daily for five days. A reverse-phase high-performance liquid chromatography with fluorescence detection (RP-HPLC-FLD) method was developed to determine AMO residues in albumen, yolk and whole egg. By using pre-column derivatisation, an improved liquid–liquid extraction procedure was developed for sample preparation. AMO were extracted from eggs with acetonitrile. The extract solution was extracted using saturated methylene chloride. The supernatant was reacted with salicylaldehyde under acidic and heating conditions. Limits of detection (LODs) were 1.2 ng g–1 and limits of quantification (LOQs) were 3.9 ng g–1 for AMO. Recoveries of AMO from samples fortified at levels of 5.0–125.0 ng g–1 ranged from 79.1% to 88.5% in albumen, 78.6–83.6% in yolk and 78.3–85.1% in whole egg, with coefficients of variation of ≤7.3%. The maximum concentrations of AMO in albumen, yolk and whole egg were found to occur at 1.5, 2.5, 1.5 days after withdrawal of medication respectively. AMO was not detectable in albumen at 7.5 days after final administration of AMO, at 10.5–11.5 days in yolk and 10.5 days in whole egg after administration of two oral doses. The method was applied during the residue study of AMO in order to formulate a reasonable withdrawal period to ensure food safety. 相似文献
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Determination of residues of deltamethrin in milk and butter 总被引:1,自引:0,他引:1
A method is described for the determination of deltamethrin, particularly in mild and dairy products. Residues and fat were co-extracted with acetone and light petroleum, partitioned with acetonitrile-methylene chloride and centrifuged (-10 degrees C). The extract was purified by gel permeation chromatography. A Florisil clean-up method was tested but did not seem effective enough. Analysis was performed by gas-liquid chromatography with a 63Ni electron-capture detector on 3% SE-30 using a short column (40 cm). Confirmation was effected by gas chromatography-mass spectrometry with an SE-30 capillary column (10 m). Recoveries from fortified samples ranged from 72 to 88% for milk spiked with 0.06 ppm and butter spiked with 2 ppm and was 94% for milk spiked with 0.016 ppm of deltamethrin. 相似文献
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建立了HPLC检测养殖水产品中四环素类抗生素残留的方法,采用乙酸乙酯(Imol/L) 乙酸镁(0.05mol/L) EDTA(0.001mol/L)的混合液提取样品中的四环素、土霉素、全霉素.以上述混合液-甲醇(72:28,v/v)为流动相,流速1mL/min,检测波长370hm.在0.05~1.0mg/L范围内峰面积与抗生素浓度呈良好的线性关系(r>0.99).检出限分别为0.013mg/g(土霉素)、0.016mg/g(四环素)、0.014mg/g(金霉素),平均加标回收率分别91.2%(土霉素)、88.5%(四环素)、95.6%(金霉素),精密度(RSD)小于5%. 相似文献
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拟除虫菊酯类农药是一类广谱性杀虫剂,采用乙腈浸提,固相萃取净化,建立了对5种拟除虫菊酯类农药进行定性定量多残留分析检测技术.具有操作快速,灵敏度高,回收率好的特点,达到了农药多残留快速检测的要求. 相似文献
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目的 建立气相色谱法测定大豆中甲基毒死蜱的残留量的分析方法。方法 使用乙腈萃取样品, 经中性氧化铝柱去除杂质, VF-5毛细管柱分离, 气相色谱仪定量分析甲基毒死蜱在大豆中的残留量。同时, 与SN/T 2324-2009中的方法进行对比, 考察了本方法的线性、回收率、精密度、重现性。结果 本方法中甲基毒死蜱在0.15~25.0 μg/mL范围内的线性关系良好, 曲线方程为: Y=6.6185X?0.0090, r2=0.99910, 甲基毒死蜱的检出限为0.01 mg/kg, 定量限为0.03 mg/kg, 加标回收率为89.7%~97.0%, 相对标准偏差为1.92%~5.11%。结论 与国标方法对比, 本方法灵敏度高, 定量准确, 具有简单实用、效率高、成本低等优点, 适合大豆中甲基毒死蜱残留量的检测。 相似文献
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采用荧光光度法测定了鲫鱼、鳗鱼、鲤鱼和罗非鱼肌肉组织中的环丙沙星药物残留量。样品用酸性乙腈提取,正己烷脱脂,水相在HAc-NaAc(pH4.5)缓冲溶液中,激发波长λex275nm,荧光测定波长λem450nm下用荧光光度法测定环丙沙星含量,环丙沙星的线性范围10 ̄150μg/L,相关系数r=0.9987,检出限为5μg/L。回收率为74.0% ̄90.6%。变异系数为2.96% ̄7.54%。 相似文献
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目的建立一种简单、快捷测定茶叶中草甘膦残留量的离子色谱分析方法。方法样品经水提取后使用乙腈沉淀阴离子杂质,离心后取上清液依次过Dionex OnGuardⅡRP柱和Dionex OnGuardⅡAg/H柱,经IonPac AS11-HC离子色谱柱(含AG11-HC保护住)分离,用KOH淋洗液自动发生器(EG)进行梯度淋洗,抑制器采用外加水模式,电导检测器检测。结果草甘膦在0.006~12.5 mg/L范围内线性关系良好(相关系数为0.9998),方法的检出限为0.19 mg/kg,定量限为0.64 mg/kg,回收率为80.7%~98.1%,日内精密度(n=6)为1.8%~3.4%,日间精密度(n=5)小于5%。结论该方法具有净化效果好、定量准确、灵敏快速的特点,适用于茶叶中草甘膦残留的检测确证,能达到GB 2763-2014的检测要求。 相似文献
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