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建立了食品接触材料中邻苯二甲酸酯快速筛查确证的高效液相色谱-高分辨质谱法(HPLC-LTQ-Orbi-trap/MS)。实验中采用加速溶剂萃取(ASE)法为样品前处理手段,优化了萃取溶剂、萃取温度、静态萃取时间等实验参数,提高了食品接触材料中邻苯二甲酸酯的提取效率。采用高分辨质谱有效地去除了基体干扰,通过静电场轨道阱全扫描得到的精确相对分子质量进行了化合物的定量,用离子阱的二级质谱图对未知化合物进行了进一步确证。结果表明:邻苯二甲酸酯的检测限为1 ng/mL;该方法的加标回收率为89.8%~101.3%,相对标准偏差均小于8.0%;所建立的方法简单,灵敏度高,适用于食品接触材料中邻苯二甲酸酯类增塑剂的筛查和检测。 相似文献
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建立了用超高效液相色谱-线性离子阱/静电场轨道阱组合高分辨质谱(UPLC-LTQ/Orbitrap MS)快速检测日用塑料袋中的35种致敏致癌染料的检测方法。样品经二氯甲烷超声提取后,用ACQUITY UPLC BEH C18色谱柱分离目标物,在m/z为150~1000范围内进行一级质谱全扫描。以准分子离子峰的精确质量数和提取的色谱图峰面积进行筛查分析和定量,以保留时间和数据依赖扫描(data-dependent scan)模式获得的子离子质谱图进行定性确证。35种致敏致癌染料的质量偏差不大于5×10~(-6)(5ppm),方法检出限为0.02 mg/kg~0.3 mg/kg,精密度(RSD)为3.5%-9.2%。 相似文献
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本文建立了高效液相色谱-串联质谱法(LC-MS/MS)同时测定猪肉中44种兽药残留的检测方法。样品中的4种四环素类、16种喹诺酮类、24种磺胺类化合物用1%甲酸乙腈溶液提取后,经QuEChERS净化,氮吹浓缩后通过C18色谱柱分离,并采用基质标准曲线法定量。结果表明44种化合物在2.0~100.0μg/kg范围内线性关系良好,相关系数R均大于0.995,加标回收率在70.8%~106.2%之间,相对标准偏差为1.1%~8.1%(n=6)。该方法操作简便、经济快速、灵敏准确,适用于猪肉中多种兽药残留的快速筛查。 相似文献
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《福建分析测试》2020,(3)
建立了用超高效液相色谱-串联质谱法快速筛查和准确定量面膜中可能非法添加的41种糖皮质激素的分析方法。样品经甲醇提取后,用Thermo Hypersil GOLD色谱柱分离目标物,以0.1%乙酸水溶液-0.1%乙酸乙腈溶液为流动相进行梯度洗脱分离,电喷雾电离(ESI),多反应监测(MRM)模式测定41种糖皮质激素,以保留时间和离子对(母离子和2个碎片子离子)信息比较进行定性,以母离子和响应值高的碎片离子外标法定量。在该方法条件下,41种糖皮质激素分离度良好,方法检出限(LOD)为0.49~1.65μg/kg,定量限(LOQ)为1.63~5.50μg/kg,回收率为82.6~118.2%,精密度为2.3~6.8%。该方法简便、准确、快速、灵敏度高,可作为面膜中非法添加糖皮质激素成分筛查和定量检测方法。 相似文献
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建立了一种用于饲料中三聚氰胺类有机物含量的气相色谱——质谱联用检测方法。通过甲醇/水/三乙胺混合液提取饲料中的三聚氰胺类有机物,氮气吹干、硅烷化衍生,再由气相色谱——质谱联用仪检测,苯代三聚氰胺内标法定量。该方法在饲料中三聚氰胺类有机物的加标回收率在82.0%-107.0%之间,相对标准偏差(RSD)不大于10.5%,在0.05mg/L-50.0mg/L范围内呈现良好的线性关系,灵敏度高,最低检测限达到10μg/kg;选择性好,能有效消除复杂基体干扰。可作为常见样品中三聚氰胺类有机物含量检测的确证方法。 相似文献
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利用紫外-可见吸收光谱,研究了一种含4个己氧基偶氮苯液晶基元的星型液晶化合物SiC6在氯仿和四氢呋喃溶液中的摩尔吸光系数、量子产率和反-顺光异构光反应,实验结果表明样品在各溶液的光致变色反应均为一级动力学反应,并求算了光致变色反应的反-顺光异构反应速率常数均为10-1数量级,远远大于偶氮类侧链液晶高分子在相同溶液中的光致变色速率常数. 相似文献
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Contemporary approaches to developing effective procedures of measurement and monitoring are considered. A justification is given for solving these problems using the method of statistical modeling. 相似文献
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An optimum policy for the warrants for and the design of guardrails based on benefit maximizing criteria is presented. It is shown that the strength, the number of classes of standards, and the location of guardrails should be determined simultaneously with due consideration for the nation-wide distribution of roadside dangers and the impact of colliding vehicles. Dynamic programming is used for optimization. 相似文献
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船舶与集装箱用钢板预处理过程中所用磨料的对比 总被引:4,自引:0,他引:4
对船舶与集装箱用钢板涂装前预处理过程中,抛(喷)丸清理(除锈、刻蚀)用各种磨料的性质、磨料硬度与侵入性及耐久性(寿命)的关系、磨料的形状与清理效果的关系、磨料的粒度与覆盖率、冲击功的关系作了对比分析,提出了合理选用磨料的原则。 相似文献
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The work package two of the ORAMED project--Collaborative Project (2008-2011) supported by the European Commission within its seventh Framework Programme--is devoted to the study of the eye lens dosimetry. A first approach is to implement the use of H(p)(3) by providing new sets of conversion coefficients and well suited calibration and type test procedures. This approach is presented in other papers in the proceedings of this conference. Taking into account that the eye lens is an organ close to the surface of the body, another approach would be to directly estimate the absorbed dose to the eye lens, D(lens,est) through a special calibration procedure although this quantity is not directly measurable. This paper is a methodological paper that tries to identify the critical aspects of a dosimetry in terms of D(lens). 相似文献
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It is shown that user-oriented software plays an important role in the design of sensor systems. Justification is provided for functional modules that make it possible to introduce instrumentation support and application shells into the sphere of metrological practice.Translated from Izmeritel'naya Tekhnika, No. 11, pp. 13–16, November, 1995. 相似文献
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This paper reviews systematic studies aimed at developing the physicochemical foundations of adsorption purification of volatile compounds of Group II–VI elements (halides, inorganic hydrides, metalorganic compounds, and process gases) attractive for electronic and optical applications. The efficiency of fine purification via adsorption is analyzed in comparison with distillation, extraction, and crystallization, and the role of the adsorption step in integrated processes for the preparation of high-purity substances is discussed. Future directions in developing adsorption techniques for fine purification of substances are outlined. 相似文献