使用氰丙基柱从血浆中简单灵敏地固相萃取百草枯。

Simple sensitive solid-phase extraction of paraquat from plasma using cyanopropyl columns.

作者信息

Smith N B, Mathialagan S, Brooks K E

机构信息

Department of Clinical Biochemistry, University Hospital, London, ON, Canada.

出版信息

J Anal Toxicol. 1993 May-Jun;17(3):143-5. doi: 10.1093/jat/17.3.143.

DOI:10.1093/jat/17.3.143

PMID:8336487

Abstract

We report an inexpensive, sensitive paraquat quantitation method which is simple to perform. First, 5 mL of blanks, standards, or patient plasma are applied to 1-mL cyanopropyl extraction columns equipped with 15-mL reservoirs. The samples are drawn through the columns under vacuum, followed by a rinse with 15-20 mL of 0.1M NH4OH. Paraquat is eluted with 0.8 mL 0.1M HCl, which is then neutralized with 25 microL concentrated NH4OH. Sodium dithionite reagent (0.23M in 4M NaOH) is added (100 microL) and the color produced is measured by absorbance difference (A395-A460). The assay is linear up to at least 4.35 microM paraquat. The lower limit of quantitation is 0.23 microM. Lipemic and icteric sera do not affect the method, but easily visible hemolysis elevates the concentrations measured by up to 0.7 microM, independent of paraquat concentration. Equimolar amounts of diquat with paraquat, at paraquat concentrations from 0.4 to 4.0 microM, elevate apparent paraquat concentrations by 0.08-0.28 microM. At 0.632, 1.92, and 4.06 microM paraquat, within-run coefficients of variation (CVs) were 6.27, 7.23, and 2.14%, and between-run CVs were 6.82, 8.42, and 4.43%, respectively.

摘要

我们报告了一种成本低廉、灵敏度高且操作简单的百草枯定量方法。首先，将5 mL空白样品、标准品或患者血浆加至配有15 mL储液器的1 mL氰丙基萃取柱中。在真空条件下将样品抽吸通过柱子，随后用15 - 20 mL 0.1M氢氧化铵冲洗。用0.8 mL 0.1M盐酸洗脱百草枯，然后用25 μL浓氢氧化铵中和。加入连二亚硫酸钠试剂（在4M氢氧化钠中为0.23M，100 μL），通过吸光度差值（A395 - A460）测量产生的颜色。该测定法在百草枯浓度至少达4.35 μM时呈线性。定量下限为0.23 μM。脂血和黄疸血清不影响该方法，但明显的溶血会使测得的浓度升高多达0.7 μM，且与百草枯浓度无关。在百草枯浓度为0.4至4.0 μM时，等摩尔量的敌草快与百草枯会使表观百草枯浓度升高0.08 - 0.28 μM。在百草枯浓度为0.632、1.92和4.06 μM时，批内变异系数（CV）分别为6.27%、7.23%和2.14%，批间CV分别为6.82%、8.42%和4.43%。