Navigation Links
Fast Analysis of Phenoxyacetic and Phenoxypropionic Herbicides in Vegetable Matrix by Negative Ion Electrospray LC/MS/MS

P.Y. Communal and A. Royer, Girpa, Angers, France
C. Schauber and T. Faye, Varian, Inc., France


Phenoxy acids are used as herbicides in agricultural and domestic areas. These compounds have to be detected at trace level to ensure a safe drinking water and food supply and verify appropriate remediation of these pollutants from contaminated sites.

Among the analytical methods developed, LC/UV exhibits poor sensitivity and inadequate selectivity for complex vegetable matrices. Negative ion ESI LC/MS has exceptionally high sensitivity for these herbicides and, with the added selectivity of MS/MS, provides accurate analyses even for the most complex sample matrices.

A highly sensitive and fast method is described below for high throughput identification and quantitation four common herbicides in vegetable extracts (Figure 1).


Varian ProStar 410 AutoSampler

Varian ProStar 210 Solvent Delivery Modules

Varian 1200L LC/MS with ESI source

Materials and Reagents

Standard solutions: pesticides were provided by the GIRPA group, France. ASE 300 (Dionex)

Florisil (Carlo Erba)

Hydromatrix bulk material (Varian Part No. 198003)

All other chemicals are reagent grade or HPLC grade.

Sample Preparation and Extraction

Liquid/solid extraction is performed using the Varian Sample Preparation Products Hydromatrix (25g) and matrix (25g onion). Two grams of Florisil is added to the homogeneous mixture followed by Accelerated Solvent Extraction (ASE) with ethyl acetate (100 mL, 100 bar, 50 0C). After 100 μL of ndodecane is added to the extract, the solution is evaporated to dryness and the residue is dissolved wi th 25 mL of acetonitrile. The final solution is then spiked with 5 ppb of herbicides.

Results and Discussion

The MS/MS conditions shown above are determined with the Automated MS/MS Breakdown software (also see Varian LC/MS Application Note 11 and 12).

The LC method uses a fast gradient program for a complete analysis in less than ten minutes. Due to the structural similarity of the acidic herbicides, incomplete resolution is observed under faster separation conditions.

The relative selectivity of LC/MS (SIM mode) and LC/MS/MS (MRM mode) are directly compared using spiked matrix samples. For pure standards, the sensitivity in the SIM mode is excellent, but even at the highest spiked concentration of 5 ppb, matrix interferences are strong. In Figure 2, SIM plots for all four herbicides shows extra peaks and baseline instability. For mecoprop, an interfering peak clearly overlaps with the analyte. As with a LC/UV detector, reliable quantitation is not possible with SIM, especially at lower concentrations.

Using the same spiked matrix extract, the increased selectivity of MS/MS is readily apparent. The MRM chromatograms in Figure 3 are interference free. The baseline is clear from any false positive peaks and no cross talk effect is observed when similar product ions are monitored in the same segment time (Table 1 and Figure 3). With the elimination of these matrix interferences, quantitation with high confidence is possible.

The MRM method has excellent linearity for all the herbicides from 0.1 to 5 ppb as shown for dichlorprop in Figure 4. The developed MRM method is also very sensitive with a LOD of 0.1 ppb for all the pesticides under the described instrument conditions.


This 1200L LC/MS/MS method is simple, fast, and hig hly sensitive. The method can quantitatively analyze pesticides at sub-ppb levels and maintain accuracy even with complex matrices. The 1200L LC/MS/MS system is recommended when sensitivity and selectivity are required at very low concentration.



Page: All 1 2 3

Related biology technology :

1. A Positive Selection Assay for Mutation Analysis in Big Blue Animals
2. Epitope-Tagging Vectors for Functional Analysis in Yeast
3. Map and Link Human Genetic Disorders with SSLP Analysis
4. CastAway Precast Gels for Rapid Automated DNA Sequence Analysis
5. Single-cell RT-PCR Analysis of Paramecium Primaurelia with the Eppendorf cMaster RTplusPCR System
6. Structural Analysis of Glycosylated Peptides in Complex Mixtures with Ion Trap MSn
7. Use of Transcriptor Reverse Transcriptase in Microarray Analysis
8. Increased Sensitivity in Microarray Analysis
9. Gene-Expression Analysis of TP, DPD, and TS Using the LightCycler mRNA Quantification KitsPLUS
10. Agilent 2100 Bioanalyzer Automated Analysis System
11. Analysis of Microarray Data
Post Your Comments:

(Date:6/27/2016)... ON , June 27, 2016 /PRNewswire/ - BIOREM Inc. ... has been advised by its major shareholders, Clean Technology ... United States based venture capital ... shares of Biorem (on a fully diluted, as converted ... the disposition of their entire equity holdings in Biorem ...
(Date:6/27/2016)... ... 27, 2016 , ... Newly created 4Sight Medical Solutions ... the healthcare market. The company's primary focus is on new product introductions, to ... that are necessary to help companies efficiently bring their products to market. , ...
(Date:6/24/2016)... , June 24, 2016  Regular discussions on a ... take place between the two entities said Poloz. ... Ottawa , he pointed to the country,s ... the federal government. ... said, "Both institutions have common economic goals, why not sit ...
(Date:6/23/2016)... ... June 23, 2016 , ... Mosio, a leader in clinical ... Patient Recruitment and Retention Tips.” Partnering with experienced clinical research professionals, Mosio revisits ... tips, tools, and strategies for clinical researchers. , “The landscape of how patients ...
Breaking Biology Technology:
(Date:4/15/2016)... 2016 Research and Markets has ... Market 2016-2020,"  report to their offering.  , ... ,The global gait biometrics market is expected to ... period 2016-2020. Gait analysis generates multiple ... used to compute factors that are not or ...
(Date:3/31/2016)... 2016  Genomics firm Nabsys has completed a financial ... Bready , M.D., who returned to the company in ... leadership team, including Chief Technology Officer, John Oliver ... Nurnberg and Vice President of Software and Informatics, ... Dr. Bready served as CEO of Nabsys from ...
(Date:3/22/2016)... Ontario , PROVO and ... Newborn Screening Ontario (NSO), which operates the ... for molecular testing, and Tute Genomics and UNIConnect, ... management technology respectively, today announced the launch of a ... next-generation sequencing (NGS) testing panel. NSO ...
Breaking Biology News(10 mins):