Method of detecting and quantifying perchlorate contamination

Patent metadata

Field	Value
Publication number	US-9664645-B2
Application number	US-201414548394-A
Country	US
Kind code	B2
Filing date	Nov 20, 2014
Priority date	Nov 20, 2014
Publication date	May 30, 2017
Grant date	May 30, 2017

Abstract

A method of detecting and quantifying perchlorate contamination in samples, especially samples with complex background matrices such as food and produce with trace levels of perchlorate. A simple microwave assisted-electromembrane extraction provides simultaneous reduced extraction time, sample clean-up, high recovery and enrichment of perchlorate ions for detection and quantification by ion chromatography. Three parallel EME experiments connected to a single DC power supply improves the precision of the analyses. It also couples well with the multiple microwave digested samples and this reduces the sample preparation time and is hence suitable for routine environmental applications.

First claim

The invention claimed is:

1. A method of detecting and quantifying perchlorate ions in a sample, comprising:
digesting the sample with an acid to form a sample solution;
heating the sample solution in a solvent with a microwave digestion system to form a microwave-digested sample;
extracting the perchlorate ions from the microwave-extracted sample with a parallel electromembrane extraction system by electromigration of the perchlorate ions across a membrane impregnated with a solvent; and
quantifying the perchlorate ions by ion chromatography;
wherein the electromembrane extraction system comprises three extraction setups connected parallel to a DC power supply and arranged in a single run.

2. The method of claim 1 , wherein the heating is carried out for 10-15 min.

3. The method of claim 1 , wherein the heating is carried out at a temperature of 60-150° C.

4. The method of claim 1 , wherein the heating is carried out at 200-250 W.

5. The method of claim 1 , wherein the heating is carried out at 20-50 V.

6. The method of claim 1 , wherein the extracting is carried out for 10-15 min.

7. The method of claim 1 , wherein the method has a limit of detection of lower than 0.05 μg per 1 g of the sample, based on a signal/noise ratio of 3.

8. The method of claim 1 , wherein the method has a limit of detection of 0.04 μg per 1 g of the sample, based on a signal/noise ratio of 3.

9. The method of claim 1 , wherein the method has a limit of quantitation of lower than 0.15 μg per 1 g of the sample, based on a signal/noise ratio of 10.

10. The method of claim 1 , wherein the method has a limit of quantitation of 0.125 μg per 1 g of the sample, based on a signal/noise ratio of 10.

11. The method of claim 1 , wherein the solvent is selected from the group consisting of 1-hexanol, 1-octanol, 1-heptanol, 1-butyl-3-methylimidazolium tetrafluoroborate, 1-butyl-3-methylimidazolium octylsulfate and 1-butyl-3-methylimidazolium hexafluorophosphate.

12. The method of claim 1 , wherein the solvent is 1-hexanol.

13. The method of claim 1 , wherein the sample has a complex background matrix.

14. The method of claim 1 , wherein the sample is selected from the group consisting of a pharmaceutical sample, a clinical sample, a chemical sample, an environmental sample, produce and food.

15. The method of claim 1 , wherein the method provides mean perchlorate recovery of greater than 95%.

Assignees

• Univ King Fahd Pet & Minerals

Inventors

• Chanbasha Basheer
• Nsubuga Hakimu

Classifications

• G01N30/96

  using ion-exchange (G01N30/02, G01N30/90 take precedence) · CPC title

• G01N33/12 Primary

  Meat; Fish · CPC title

• G01N27/447 Primary

  using electrophoresis · CPC title

• B01D15/36

  involving ionic interaction, e.g. ion-exchange, ion-pair, ion-suppression or ion-exclusion · CPC title

• B01D61/52

  Accessories; Auxiliary operation · CPC title