Suppr超能文献

建立超高压液相色谱-串联质谱法检测多种磺胺类药物残留的分析方法,并应用于猪养殖场所水样、粪浆和土壤中磺胺类药物的检测。

Development of an ultra-high-pressure liquid chromatography-tandem mass spectrometry multi-residue sulfonamide method and its application to water, manure slurry, and soils from swine rearing facilities.

机构信息

USDA-ARS, Biosciences Research Laboratory, 1605 Albrecht Boulevard, Fargo, ND 58105, USA.

出版信息

J Chromatogr A. 2010 Feb 19;1217(8):1273-82. doi: 10.1016/j.chroma.2009.12.034. Epub 2009 Dec 16.

Abstract

An analytical method was developed using ultra-high-pressure liquid chromatography-triple quadrupole-tandem mass spectrometry (UHPLC-TQ-MS/MS) to simultaneously analyze 14 sulfonamides (SA) in 6 min. Despite the rapidity of the assay the system was properly re-equilibrated in this time. No carryover was observed even after high analyte concentrations. The instrumental detection limit based on signal-to-noise ratio (S/N)>3, was below 1 pg/microL (5 pg on column) for all SAs except sulfachloropyridazine. Surface water, ground water, soil, and slurry manure contained in storage ponds in and around swine [Sus scrofa domesticus] rearing facilities were analyzed. Sample cleanup for ground water and surface water included using solid phase extraction (SPE) using Oasis hydrophilic-lipophilic balance (HLB) cartridges. The soil and slurry manure required tandem strong anion exchange (SAX) and HLB solid phase extraction cartridges for sample cleanup. With few exceptions, the recoveries ranged from 60 to 100% for all matrices. The minimum detectable levels were below 2.0 ng/L for water, 30 ng/L for slurry manure, and 45 ng/kg for soil except for sulfachloropyridazine. The coefficient of variation (CV) was within 20% for most of the compounds analyzed. Using this method, sulfamethazine concentrations of 2250-5060 ng/L, sulfamethoxazole concentrations of 108-1.47 x 10(6)ng/L, and sulfathiazole concentrations of 785-1700 ng/L were found in the slurry manure. Sulfadimethoxine (2.0-32 ng/L), sulfamethazine (2.0-5.1 ng/L), and sulfamethoxazole (20.5-43.0 ng/L) were found in surface water and ground water. In top soil (0-15 cm), sulfamethazine ranged 34.5-663 ng/kg dry weight in those locations that received slurry manure as a nutrient; no SAs were found in the soil depths between 46 and 61 cm. The speed makes the method practical for medium to high throughput applications. The sensitivity and positive analyte identification make the method suitable for the demanding requirements for real world applications.

摘要

建立了一种超高效液相色谱-三重四极杆串联质谱法(UHPLC-TQ-MS/MS)同时分析 6min 内 14 种磺胺类药物(SA)的分析方法。尽管分析速度很快,但系统在这段时间内得到了适当的重新平衡。即使在高分析物浓度下也没有观察到交叉污染。基于信噪比(S/N)>3 的仪器检测限,除磺胺氯哒嗪外,所有磺胺类药物的检测限均低于 1pg/μL(5pg 柱上)。对来自养猪场(Sus scrofa domesticus)及其周围的地表水、地下水、土壤和储存在储存池中的粪便进行了分析。地下水和地表水的样品净化包括使用 Oasis 亲水亲脂平衡(HLB)小柱进行固相萃取(SPE)。土壤和粪便需要串联强阴离子交换(SAX)和 HLB 固相萃取小柱进行样品净化。除磺胺氯哒嗪外,所有基质的回收率均在 60%至 100%之间。除磺胺氯哒嗪外,水的最低检测水平均低于 2.0ng/L,粪便的最低检测水平均低于 30ng/L,土壤的最低检测水平均低于 45ng/kg。大多数分析化合物的变异系数(CV)在 20%以内。使用该方法,在粪便中发现磺胺嘧啶浓度为 2250-5060ng/L,磺胺甲恶唑浓度为 108-1.47×10(6)ng/L,磺胺噻唑浓度为 785-1700ng/L。在地表水和地下水中发现磺胺二甲氧嘧啶(2.0-32ng/L)、磺胺嘧啶(2.0-5.1ng/L)和磺胺甲恶唑(20.5-43.0ng/L)。在表层土壤(0-15cm)中,在接收粪便作为养分的位置,磺胺嘧啶浓度范围为 34.5-663ng/kg 干重;在 46-61cm 之间的土壤深度未发现任何磺胺类药物。该方法的速度使其适用于中高通量应用。该方法的灵敏度和阳性分析物鉴定使其适用于实际应用的苛刻要求。

文献AI研究员

20分钟写一篇综述,助力文献阅读效率提升50倍。

立即体验

用中文搜PubMed

大模型驱动的PubMed中文搜索引擎

马上搜索

文档翻译

学术文献翻译模型,支持多种主流文档格式。

立即体验