Supported liquid extraction offers improved sample preparation for aldosterone analysis by liquid chromatography tandem mass spectrometry

2012 ◽  
Vol 65 (11) ◽  
pp. 1045-1048 ◽  
Author(s):  
Jessica Grace Van Der Gugten ◽  
Matthew Crawford ◽  
Russell P Grant ◽  
Daniel T Holmes

BackgroundTo evaluate the accuracy and precision of a method for serum aldosterone using supported liquid extraction (SLE) for sample preparation instead of the more conventional liquid-liquid extraction (LLE) approach.MethodsTwo independently developed SLE-based LC-MS/MS methods for serum aldosterone (sample volumes 250 μl and 300 μl respectively) were compared to a modification of a previously reported LLE approach (sample volume 500 μl) in two method comparisons (n=75 and n=97). SLE analyses were performed at two separate centres. Precision was evaluated at a single site using human pools in head-to-head comparison between SLE and LLE. All analyses were performed on the ABSCIEX API-5000 LC-MS/MS system.ResultsAt four increasing pool concentrations spanning 67-1060 pmol/l, total precision for SLE ranged from 6.8-4.1% compared with 11.1-4.3% for LLE. Differences did not reach statistical significance except at the lowest concentration where SLE was superior. Pasing Bablok regression comparisons were SLE=0.96×LLE-5.8 pmol/l (R2=0.985) and SLE=0.96×LLE-0.44 pmol/l (R2=0.969).ConclusionsFor analysis of serum aldosterone on the ABSCIEX API-5000, SLE affords a smaller sample volume while maintaining the accuracy and precision performance of LLE. By avoiding specimen vortexing, SLE also allows for greater automation in the sample preparation.

Author(s):  
Ana Carolina Furiozo Arantes ◽  
Kelly Francisco da Cunha ◽  
Marilia Santoro Cardoso ◽  
Karina Diniz Oliveira ◽  
Jose Luiz Costa

Abstract Purpose We developed and validated a method for quantitative analysis of 50 psychoactive substances and metabolites (antidepressants, benzodiazepines and opioids) in oral fluid samples using simple liquid–liquid extraction procedure followed by liquid chromatography–tandem mass spectrometry (LC–MS/MS). Method Oral fluid samples were collected using Quantisal™ device and extracted by liquid–liquid extraction with 1.0 mL of methyl tert-butyl ether and then analyzed using LC–MS/MS. Results The method attended method validation criteria, with limits of quantification as low as 0.5 and 1.0 ng/mL, and linearity between 0.5–50.0 ng/mL for antidepressants, 0.5–25.0 ng/mL for benzodiazepines and 1.0–50.0 ng/mL to opioids. During method validation, bias and imprecision values were not greater than 16 and 20%, respectively. Ionization suppression/enhancement bias results were not greater than 25%. No evidence of carryover was observed. Sample stability studies showed that almost all analytes were stable at 25 °C for 3 days and at 4 °C for 7 days. Freeze–thaw cycles stability showed that most antidepressants and opioids were stable under these conditions. Autosampler stability study showed that all analytes were stable for 24 h, except for nitrazepam and 7-aminoclonazepam. Thirty-eight authentic oral fluid samples were analyzed; 36.8% of the samples were positive for 2 drugs. Citalopram was the most common drug found, followed by venlafaxine. Conclusions The method was validated according to international recommendations for the 50 analytes, showing low limits of quantification, good imprecision and bias values, using simple liquid–liquid extraction, and was successfully applied to authentic oral fluid samples analysis.


Molecules ◽  
2020 ◽  
Vol 25 (4) ◽  
pp. 987 ◽  
Author(s):  
Bo Wang ◽  
Jianyu Liu ◽  
Xia Zhao ◽  
Kaizhou Xie ◽  
Zhixiang Diao ◽  
...  

A method for the simultaneous determination of robenidine, halofuginone, lasalocid, monensin, nigericin, salinomycin, narasin, and maduramicin residues in eggs by liquid chromatography–tandem mass spectrometry (LC–MS/MS) was developed. The sample preparation method used a combination of liquid–liquid extraction (LLE) and solid-phase extraction (SPE) technology to extract and purify these target compounds from eggs. The target compounds were separated by gradient elution using high-performance liquid chromatography (HPLC) and ultra-performance liquid chromatography (UPLC). Tandem mass spectrometry was used to quantitatively and qualitatively analyze the target compounds via electrospray ionization (ESI+) and multiple reaction monitoring mode. The HPLC–MS/MS and UPLC–MS/MS methods were validated according to the requirements defined by the European Union and the Food and Drug Administration. The limits of detection and limits of quantification of the eight coccidiostats in eggs were 0.23–0.52 µg/kg and 0.82–1.73 µg/kg for HPLC–MS/MS, and 0.16-0.42 µg/kg and 0.81-1.25 µg/kg for UPLC–MS/MS, respectively. The eggs were spiked with four concentrations of the eight coccidiostats, and the HPLC–MS/MS and UPLC–MS/MS average recoveries were all higher than 71.69% and 72.26%, respectively. Compared with the HPLC–MS/MS method, utilizing UPLC–MS/MS had the advantages of low reagent consumption, a short detection time, and high recovery and precision. Finally, the HPLC–MS/MS and UPLC–MS/MS methods were successfully applied to detect eight coccidiostats in 40 eggs.


Sign in / Sign up

Export Citation Format

Share Document