Method Package for Water Quality Analysis

Method Package for Water Quality Analysis (Golf Course Pesticides and Pesticides Targeted for Water Quality Control)

Concern about many of the pesticides used to maintain the turf at golf courses exists because of the possibility of contamination of nearby fresh water sources and tap water. The "Provisional Guidance Indicators for the Prevention of Water Pollution from Pesticides Used in Golf Courses" was originally published by Japan's Ministry of the Environment in 1990. In a related notification issued on September 29, 2010, indicator values for 72 pesticides were specified, and 44 pesticides were targeted for evaluation using LC/MS.

In addition, there is significant concern over pesticides in tap water, leading to the establishment of water quality control target setting items. 31 pesticides are currently targeted in the "Attached Method 18 – Simultaneous Analysis Using Solid-Phase Extraction – Liquid Chromatograph - Mass Spectrometer" for the water quality control target setting items (revised in April 2010)

In this method package, analytical conditions and compound data are registered with respect to golf course pesticides (44 pesticides), and pesticides targeted for water quality control (30 pesticides excluding oxine-copper, plus simazine and tiobencarb, for a total of 32 pesticides). This package enables analysis without the troublesome process of investigating the separation conditions required for LCMSMS analysis, or optimization of the MS parameters for each of the target compounds. As a result, batch analysis of multiple components can be efficiently performed.

Analysis Example

Measurements of golf course wastewater were performed. MRM chromatograms (simazine, diazinon, isoxathion, and triflumizole as examples) are shown for sample solutions (no standard samples added), and sample solutions with either 10 μg/L or 50 μg/L of standard samples added. In the wastewater used here, no pesticides were detected. However in the sample solutions with the standard samples added, the concentrations at 1/3 to 1/10 of the indicator values were all detected with excellent S/N ratios, and no interference from contaminating components.

No standard samples added

Standard samples added

In addition, an example is shown of the analysis of 32 pesticides targeted for water quality control using this method package. Excellent repeatability and linearity were obtained over 6 consecutive analyses of the standard samples for each pesticide. Quantitative limits falling below 5 times the target value concentrations are also shown for all of the components. (In actual sample analysis, during pretreatment, samples are concentrated 500 times with solid-phase columns. In reality, detection of 5 times the target value concentration is required in order to detect 1/100 of the target value concentration.)

List of Registered Compounds

Analytical Conditions

Golf Course Pesticides
Analysis Column Shim-pack XR-ODSII(150mmL. x2.0mmI.D. , 2.2μm)
Mobile Phase A 5mmol/L ammonium acetate - Water
Mobile Phase B 5mmol/L ammonium acetate - Methanol
Flow Rate 0.2mL/min (gradient elution)
Injection Volume 5μL
Oven Temperature 40℃
Pesticides Targeted for Water Quality Control
Analysis Column L-Column ODS(150mmL. x2.1mmI.D. , 5μm)
Mobile Phase A 0.1% formic acid - Water
Mobile Phase B Acetonitrile
Flow Rate 0.2mL/min (gradient elution)
Injection Volume 10μL
Oven Temperature 40℃


Applicable model: LCMS-8030, LCMS-8040, LCMS-8050

Workstation: LabSolutions LCMS Ver.5.41 or later

Product components: Method files, report format files, method parameter list (text file containing measurement parameters for each component)

Remarks and Precautions

  1. Shimadzu makes no warranty regarding the accuracy of information included in the database or the usefulness of information obtained from using the database.

  2. Be sure to perform tests using standard samples to confirm qualitative and quantitative information obtained with the given system.

  3. To reliably identify registered substances using this database, measure samples using the instrument parameters specified in the method template files included in the product.

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