共查询到17条相似文献,搜索用时 109 毫秒
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本文建立了介质阻挡放电电离结合小型便携式质谱法现场快速筛查喷雾化妆品中禁用物质。介质阻挡放电电离源以石英管作为介质阻挡,以氦气为载气,流速220 mL/min。将电离源置于小型便携式质谱仪进样口前端3 cm处,喷雾化妆品样品位于电离源正上方8 cm处。样品无需前处理,按正常使用方法按压染发喷雾剂和喷雾化妆水样品喷雾阀,产生的样品微滴与介质阻挡放电电离源产生的等离子体束发生碰撞和电荷转移,实现目标化合物的离子化。结合小型便携式质谱仪,实现了染发喷雾剂中4种禁用着色剂和喷雾化妆水中4种禁用芳香剂的现场快速筛查,检出限在10~50μg/kg之间,检测时间小于1 min。该方法简便、快速、高效,适用于喷雾化妆品中禁用物质的现场快速筛查。 相似文献
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以铝基硅胶薄层板作为纸喷雾离子源基底材料,结合小型便携式质谱建立了血液样品中他克莫司、西罗莫司、依维莫司、环孢素A和霉酚酸等5种免疫抑制剂的即时检验方法。将铝基硅胶薄层板剪成三角形,滴加10μL血液样品,以20μL甲醇作为洗脱/喷雾溶剂,薄层板尖端距离小型便携式质谱进样口1.0 cm,施加喷雾电压,样品在薄层板上洗脱后形成电喷雾,进入小型便携式质谱进行分析。结果表明,5种免疫抑制剂在各自的线性范围内呈现良好的线性关系,相关系数(r)为0.993 9~0.996 8,检出限和定量限分别为0.5~5、1~10 mg/L。在低、中、高3个加标浓度水平下,平均回收率在91.0%~114.3%之间,相对标准偏差(RSD)小于8.4%,检测周期小于1 min。该方法简单快速、准确高效,适用于血液中免疫抑制剂的即时床旁分析。 相似文献
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建立了香水中邻苯二甲酸酯的快速检测方法。采用电喷雾萃取电离技术(EESI)对5种不同品牌香水中邻苯二甲酸二乙酯(DEP)进行了快速直接质谱分析。结果表明:电喷雾萃取电离质谱(EESI-MS)法能够定性定量分析香水中DEP,线性范围为20~1 000 μg/L,线性相关系数R2为0.988 9,检出限为0.39 μg/L,定量限为5.47 μg/L,回收率为94.8%~103.4%,相对标准偏差为1.5%~4.1%。该方法具有检出限低、准确度高、分析速度快(单个样品的测定时间小于30 s)、无需复杂的样品预处理等优点,可为香水中邻苯二甲酸酯的快速检测提供方法参考。 相似文献
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《分析仪器》2017,(6)
建立了测定复杂基体中壬基酚(Nonylphenol,NP)的快速溶剂萃取-在线固相萃取/高效液相色谱串联质谱分析方法。污泥、土壤及植物样品经冷冻干燥后,用正己烷、二氯甲烷、甲醇的混合溶剂(8∶1∶1,v/v/v)进行快速溶剂萃取;萃取液采用Spark在线固相萃取装置和配套在线固相萃取小柱进行在线富集和净化,以甲醇-0.1%氨水为流动相进行梯度洗脱,采用Agilent Poroshell 120EC-C18高效液相色谱柱进行分离和分析。使用安捷伦6420三重四极杆串联质谱仪为质谱检测器,采用电喷雾电离源,以多反应监测(MRM)方式进行负离子模式监测,对复杂基体中NP进行定量分析。该方法 NP线性范围为0.25~75ng,相关系数r0.999,检出限为0.05ng;该方法污泥样品的回收率为67.8%~82.6%,植物样的回收率为65.9%~96.5%;随机选取样品总数的十分之一进行平行样测定,相对偏差为0.1%~24.1%。该方法操作简单、灵敏,自动化程度高,可用于复杂基体中NP的快速测定。 相似文献
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固相萃取/LC-MS/MS法检测动物源性食品中的金刚烷胺 总被引:3,自引:0,他引:3
建立测定动物源性食品中金刚烷胺的固相萃取/液相色谱一电喷雾串联质谱分析方法。以甲醇-1%三氯乙酸(50+50,v/v)作提取溶剂,采用超声波辅助溶剂萃取法萃取动物源性食品,萃取液用Waters Oasis MCX固相萃取柱进行净化浓缩。以ThermoHypersil Gold C_(18)色谱柱为分离柱,在正离子模式下以电喷雾电离串联质谱仪进行测定。对流动相组分和流动相添加剂对质谱的离子化效率进行考察,在1.0~50.0 ng/mL范围内线性关系良好(r?0.99)。样品在5.0 μg/k,10.0μg/k和20.0 μ g/kg添加水平的回收率为75.9%~108.5%,相对标准偏差小于8.0%;方法的检出限为5.0μg/kg。本方法具有很高的灵敏度和准确度,能够满足动物源性食品中的金刚烷胺残留量的快速、高灵敏检测分析。 相似文献
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Mass spectrometry (MS) is a powerful tool for the analysis of complex mixtures. We have developed a new ambient ionization method, named paper spray, to address the need for rapid methods of direct analysis of complex mixtures without sample preparation. Paper spray is applicable to the analysis of a wide variety of compounds, including small organic compounds, peptides, and proteins. Procedures are developed for analysis of dried biofluid spots with whole blood and urine samples. The combination of sample collection from surfaces and paper spray ionization also enables fast chemical screening at high sensitivity. The combination of paper spray with miniature mass spectrometers offers a powerful impetus to wide application of mass spectrometry in non-laboratory environments. 相似文献
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A method for rapid determination of narcotics by surface desorption atmospheric pressure chemical ionization mass spectrometry (DAPCI-MS) was established. The operation parameters including spray voltage, capillary temperature ect. on analysis performance were systematically investigated. Under the optimized experimental conditions, trace amounts of methamphetamine and caffeine in ice drug were detected rapidly without any sample preparation and pretreatment. Since DAPCI-MS allows rapid analyzing trace amounts of narcotics without sample pretreatment, it was also proposed to couple DAPCI source to a miniature mass spectrometer for fast in-situ analysis of narcotics. 相似文献
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This paper describes a sample inlet system with several advantages over other pulsed valves, as applied to resonance-enhanced multiphoton ionization/time-of-flight mass spectrometry. The nozzle is based on online concentration by analyte adsorption/laser desorption (online COLD), where a capillary column with a narrowly synthesized tip is employed for sample introduction. The analyte molecules adsorbed at the tip are desorbed by a pulsed laser and are injected into a mass spectrometer as a packet. The online COLD nozzle can produce very short gas pulses on the order of 1 μs. Moreover, this nozzle is capable of operating over a wide range of repetition rates from 1 Hz to 1 kHz. In addition, this nozzle intrinsically possesses several unique characteristics; for instance, it can be heated to very high temperatures and has nearly zero dead volume. Therefore, the present sample introduction technique offers an ideal and versatile nozzle for laser ionization/mass spectrometry. 相似文献
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同位素稀释-超高效液相色谱-串联质谱技术分析婴儿配方奶粉中的维生素D 总被引:1,自引:0,他引:1
为了准确测定婴儿配方奶粉中维生素D的含量,建立了同位素稀释-超高效液相色谱-串联质谱联用技术分析维生素D含量的方法。样品经氢氧化钾皂化,用V(正戊烷)∶V(乙醚)=4∶1的混合溶液提取,采用Waters T3色谱柱分离,以2 mmol/L甲酸铵-甲醇和2 mmol/L甲酸铵-水溶液为流动相进行梯度洗脱,采用电喷雾-正离子电离源多反应监测模式进行定性和定量分析,内标法定量。维生素D2和维生素D3在5~150 μg/L质量浓度范围内线性关系良好,维生素D2和维生素D3的检出限均为1.5 μg/kg,定量限均为5.0 μg/kg,方法回收率分别为97.0%~104.7%和92.7%~108.0%,日内和日间相对标准偏差均小于10%。该方法简单、灵敏度高、分析时间短、定量准确,适用于婴儿奶粉中维生素D的测定。 相似文献
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A rapid, specific and highly sensitive method for the simultaneous determination of seven sex hormones residueing in animal product was developed, which was based on UPLC-MS/MS under positive mode using electrospray ionization(ESI) source. ZnCl2 was added to the extract solution to remove fat, and then target compounds were purified by LC-C18 and LC-NH2 solid phase extraction cartridge. Average recoveries for the seven sex hormone(spiked at the levels of 4 μg kg-1 in fish product) range from 88% to 105%,with relative standard deviations between 4.3% and 24%. 相似文献