微柱快速微固相萃取-巯基化介孔二氧化硅纳米颗粒填料填料分离测定人体尿液和水中的铅

M. Gou, Baharak Bahrami Yarahmadi
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引用次数: 8

摘要

采用巯基功能化介孔二氧化硅纳米颗粒(HS-MSNPs)作为填料柱微固相萃取(PC-MSPE)提取尿、水样中的铅离子(PbII)。将15mg hs - msnp装入注射器盒(SC, 5ml)中,用纤维素膜包装,pH调节在5.5-6.5。然后,推注射器的柱塞,在hs - msnp上有效地提取尿和水样中的铅。最后用无机酸溶液反提Pb (II),剩余溶液用电热原子吸收光谱法(ET-AAS)测定。通过优化条件,5 mL尿样的富集因子为24.8,LOD为0.04 μg -1,线性范围为0.12 ~ 5.5 μg -1, RSD% < 5%。通过在水和尿样中使用经认证的标准物质(CRM, NIST)对真实样品进行峰化验证。
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Separation and determination of lead in human urine and water samples based on thiol functionalized mesoporous silica nanoparticles packed on cartridges by micro column fast micro solid-phase extraction
An efficient method based on thiol functionalized mesoporous silica nanoparticles (HS-MSNPs) was used for extraction of lead ions (PbII) from urine and water samples by packed column micro solid phase extraction (PC-MSPE). By procedure, 15 mg of HS-MSNPs packed in syringe cartridges (SC, 5 mL) with cellulose membrane and pH adjusting at 5.5-6.5.  Then, the lead of urine and water sample was efficiently extracted on HS-MSNPs after pushing the plunger of a syringe. Finally, the Pb (II) was back-extracted with inorganic acid solution and the remained solution determined by electrothermal atomic absorption spectrometry (ET-AAS). By optimization conditions, the enrichment factor, LOD, linear range and RSD% was obtained 24.8, 0.04 μg L-1, 0.12-5.5 μg L-1 and less than 5%, respectively for 5 mL of urine samples. The validation was confirmed by spiking of real samples and using certified reference material (CRM, NIST) in water and urine sample.
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