Liver residues of diphacinone in Polynesian rats and house mice offered a novel bait

Metadata:
Identification_Information:
Citation:
Citation_Information:
Originator: Goldade, David A.
Publication_Date: 2023
Title:
Liver residues of diphacinone in Polynesian rats and house mice offered a novel bait
Geospatial_Data_Presentation_Form: tabular digital data
Series_Information:
Series_Name: Research Dataset Series
Publication_Information:
Publication_Place: Fort Collins, CO
Publisher: USDA, APHIS, WS National Wildlife Research Center
Online_Linkage: https://doi.org/10.2737/NWRC-RDS-2023-002
Description:
Abstract:
Diphacinone residues in the livers of Polynesian rats and house mice that were trapped from wild populations in Hawaii and fed a novel diet formulation were determined using a dispersive solid phase extraction technique paired with tandem mass spectrometry. Data include chromatograms and data summaries collected using an Agilent 4670 QQQ mass spectrometer. Measurements were taken at the National Wildlife Research Center’s chemistry laboratory in Hawaii between June 22 and August 2 of 2022.
Purpose:
The data were collected to determine residue levels of the rodenticide diphacinone in the livers of rodents used to test the efficacy of a new bait formulation.
Supplemental_Information:
For more information about this study, see Goldade et al. (2023).

These data were published on 07/19/2023. On 03/01/2024, the metadata was updated to include more details for the recently published article.
Time_Period_of_Content:
Time_Period_Information:
Range_of_Dates/Times:
Beginning_Date: 20220622
Ending_Date: 20220802
Currentness_Reference:
Ground condition
Status:
Progress: Complete
Maintenance_and_Update_Frequency: As needed
Spatial_Domain:
Description_of_Geographic_Extent:
Polynesian rats and house mice were trapped from wild populations in Hawaii and transported to the National Wildlife Research Center’s Hawaii Field Station.
Bounding_Coordinates:
West_Bounding_Coordinate: -105.15046
East_Bounding_Coordinate: -105.15046
North_Bounding_Coordinate: 40.58619
South_Bounding_Coordinate: 40.58619
Bounding_Altitudes:
Altitude_Minimum: 1614
Altitude_Maximum: 1614
Altitude_Distance_Units: meters
Keywords:
Theme:
Theme_Keyword_Thesaurus: ISO 19115 Topic Category
Theme_Keyword: environment
Theme:
Theme_Keyword_Thesaurus: National Research & Development Taxonomy
Theme_Keyword: Wildlife (or Fauna)
Theme_Keyword: Mammals
Theme:
Theme_Keyword_Thesaurus: None
Theme_Keyword: rodenticide
Theme_Keyword: diphacinone
Theme_Keyword: Polynesian rats
Theme_Keyword: mice
Theme_Keyword: liver residue
Theme_Keyword: LC-MS-MS
Place:
Place_Keyword_Thesaurus: None
Place_Keyword: Hawaii
Taxonomy:
Keywords/Taxon:
Taxonomic_Keyword_Thesaurus:
None
Taxonomic_Keywords: multiple species
Taxonomic_Keywords: mammals
Taxonomic_System:
Classification_System/Authority:
Classification_System_Citation:
Citation_Information:
Originator: ITIS
Publication_Date: 2023
Title:
Integrated Taxonomic Information System
Geospatial_Data_Presentation_Form: on-line
Other_Citation_Details:
Retrieved [July, 14, 2023]; CC0
Online_Linkage: https://www.itis.gov
Online_Linkage: https://doi.org/10.5066/F7KH0KBK
Taxonomic_Procedures:
Taxonomic_Classification:
Taxon_Rank_Name: Kingdom
Taxon_Rank_Value: Animalia
Applicable_Common_Name: Animal
Applicable_Common_Name: animaux
Applicable_Common_Name: animals
Taxonomic_Classification:
Taxon_Rank_Name: Subkingdom
Taxon_Rank_Value: Bilateria
Applicable_Common_Name: triploblasts
Taxonomic_Classification:
Taxon_Rank_Name: Infrakingdom
Taxon_Rank_Value: Deuterostomia
Taxonomic_Classification:
Taxon_Rank_Name: Phylum
Taxon_Rank_Value: Chordata
Applicable_Common_Name: cordés
Applicable_Common_Name: cordado
Applicable_Common_Name: chordates
Taxonomic_Classification:
Taxon_Rank_Name: Subphylum
Taxon_Rank_Value: Vertebrata
Applicable_Common_Name: vertebrado
Applicable_Common_Name: vertébrés
Applicable_Common_Name: vertebrates
Taxonomic_Classification:
Taxon_Rank_Name: Infraphylum
Taxon_Rank_Value: Gnathostomata
Taxonomic_Classification:
Taxon_Rank_Name: Superclass
Taxon_Rank_Value: Tetrapoda
Taxonomic_Classification:
Taxon_Rank_Name: Class
Taxon_Rank_Value: Mammalia
Applicable_Common_Name: mammifères
Applicable_Common_Name: mamífero
Applicable_Common_Name: mammals
Taxonomic_Classification:
Taxon_Rank_Name: Subclass
Taxon_Rank_Value: Theria
Taxonomic_Classification:
Taxon_Rank_Name: Infraclass
Taxon_Rank_Value: Eutheria
Taxonomic_Classification:
Taxon_Rank_Name: Order
Taxon_Rank_Value: Rodentia
Applicable_Common_Name: esquilo
Applicable_Common_Name: preá
Applicable_Common_Name: rato
Applicable_Common_Name: roedor
Applicable_Common_Name: rongeurs
Applicable_Common_Name: rodents
Taxonomic_Classification:
Taxon_Rank_Name: Suborder
Taxon_Rank_Value: Myomorpha
Applicable_Common_Name: Rats
Applicable_Common_Name: souris
Applicable_Common_Name: Mice
Applicable_Common_Name: Rats
Applicable_Common_Name: Voles
Applicable_Common_Name: Gerbils
Applicable_Common_Name: Hamsters
Applicable_Common_Name: Lemmings
Taxonomic_Classification:
Taxon_Rank_Name: Superfamily
Taxon_Rank_Value: Muroidea
Taxonomic_Classification:
Taxon_Rank_Name: Family
Taxon_Rank_Value: Muridae
Applicable_Common_Name: campagnols
Applicable_Common_Name: rats
Applicable_Common_Name: souris
Applicable_Common_Name: mice
Applicable_Common_Name: rats
Applicable_Common_Name: voles
Taxonomic_Classification:
Taxon_Rank_Name: Subfamily
Taxon_Rank_Value: Murinae
Applicable_Common_Name: Old World rats
Applicable_Common_Name: Old World mice
Taxonomic_Classification:
Taxon_Rank_Name: Genus
Taxon_Rank_Value: Rattus
Applicable_Common_Name: Old World Rats
Taxonomic_Classification:
Taxon_Rank_Name: Species
Taxon_Rank_Value: Rattus exulans
Applicable_Common_Name: Polynesian rat
Applicable_Common_Name: Little Rat
Applicable_Common_Name: Pacific Rat
Taxonomic_Classification:
Taxon_Rank_Name: Genus
Taxon_Rank_Value: Mus
Applicable_Common_Name: House Mice
Applicable_Common_Name: Old World Mice
Taxonomic_Classification:
Taxon_Rank_Name: Subgenus
Taxon_Rank_Value: Mus (Mus)
Taxonomic_Classification:
Taxon_Rank_Name: Species
Taxon_Rank_Value: Mus musculus
Applicable_Common_Name: souris commune
Applicable_Common_Name: House Mouse
Access_Constraints: None
Use_Constraints:
These data were collected using funding from the U.S. Government and can be used without additional permissions or fees. If you use these data in a publication, presentation, or other research product please use the following citation:

Goldade, David A. 2023. Liver residues of diphacinone in Polynesian rats and house mice offered a novel bait. Research Dataset Series. USDA, APHIS, WS National Wildlife Research Center. Ft. Collins, Colorado. https://doi.org/10.2737/NWRC-RDS-2023-002
Point_of_Contact:
Contact_Information:
Contact_Organization_Primary:
Contact_Organization: USDA, APHIS, Wildlife Service, National Wildlife Research Center
Contact_Person: David A. Goldade
Contact_Position: Supervisory Chemist
Contact_Address:
Address_Type: mailing and physical
Address: 4101 LaPorte Avenue
City: Fort Collins
State_or_Province: CO
Postal_Code: 80521
Country: USA
Contact_Voice_Telephone: 970-266-6080
Contact_Electronic_Mail_Address: david.a.goldade@usda.gov
Data_Set_Credit:
This project was funded by U.S. Department of Agriculture, Animal and Plant Health Inspection Service, Wildlife Services, National Wildlife Research Center as well as Bell Laboratories.


Author Information:

David A. Goldade
USDA, APHIS, Wildlife Service, National Wildlife Research Center
https://orcid.org/0000-0003-0041-445X
Cross_Reference:
Citation_Information:
Originator: Goldade, David A.
Originator: Siers, Shane R.
Originator: Hess, Steven C.
Originator: Sugihara, Robert T.
Originator: Riekena, Craig A.
Publication_Date: 2023
Title:
Determination of residue levels of rodenticide in rodent livers offered novel diphacinone baits by liquid chromatography-tandem mass spectrometry
Geospatial_Data_Presentation_Form: journal article
Series_Information:
Series_Name: PLOS One
Issue_Identification: 18(8): e0289261
Online_Linkage: https://doi.org/10.1371/journal.pone.0289261
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Data_Quality_Information:
Attribute_Accuracy:
Attribute_Accuracy_Report:
The average precision of diphacinone (DPN), represented by the relative standard deviation of the observed concentrations, was 7.2% (range = 0.97% – 20.4%) and the average accuracy, represented by the relative error, was 5.8% (range = 1.06% - 14.7%).
Logical_Consistency_Report:
The data are logically consistent. The consistency was verified as part of the quality assurance that occurred during data analysis.
Completeness_Report:
No missing data
Lineage:
Methodology:
Methodology_Type: Field
Methodology_Description:
STUDY DESIGN

Some evidence suggests that eradications in tropical ecosystems are more prone to eradication failure. For eradications to be successful, the applied baits must be both highly efficacious and palatable to the rodents. To address potential palatability issues, novel bait matrices under development for deployment in eradication operations were formulated at 50 and 100 parts per million (ppm) diphacinone and offered to wild-caught Polynesian rats (Rattus exulans) and house mice (Mus musculus) in a two-choice test with the test animals being offered both the formulated bait and a standard maintenance diet. The livers were harvested from the mice and rats and analyzed for diphacinone residues by liquid chromatography with tandem mass spectrometry to verify bait consumption and inform potential risk assessments from secondary exposures. Ninety-two Polynesian rats (Rattus exulans) and ninety-two house mice (Mus musculus) of mixed genders were trapped from wild populations in Hawaii with no known exposure to anticoagulant rodenticides and transported to the National Wildlife Research Center’s Hawaii Field Station.

The rats and mice were randomly divided into test and control groups. On test day 0, half of the test animals were offered either a 50 or 100 ppm DPN formulated bait comprised of compressed cereal pellets with a proprietary formulation (Bell Laboratories, Madison, WI, USA). The test animals were also offered a U.S. EPA standard challenge diet in a two-choice test. Control animals received only the standard animal feed. The rodents were allowed to feed ad libitum for 15 days, followed by a 10-day holding period during which the formulated baits were removed, and all animals received only the standard animal feed diet. Consumption of bait and challenge diet (grams) was recorded daily. Twice daily, the condition of the rodents was observed and noted. Deceased animals were removed; their weight and the time were recorded. No individuals from the control group expired during the exposure period. All rodents that survived the full 15-day exposure period and 10-day post-exposure period were euthanized with CO₂. All animals were euthanized humanely in accordance with American Veterinary Medical Association standards and practices.

There were too many tissues samples to extract and analyze in a single day, therefore we broke them up into subgroups which are referenced as Part 1, Part 2, etc.


DATA COLLECTION

Liver tissue samples were extracted with a mixture of water and acetonitrile containing ammonium hydroxide. The sample was cleaned up with a combination of liquid-liquid partitioning and dispersive solid phase extraction. Separation was achieved using a Waters X-Bridge BEH C-18 LC column (50 millimeter [mm], 2.1 mm ID, 2.5 micrometer [µm] particle size) with detection on a triple quadrupole mass spectrometer in multiple reaction monitoring (MRM) mode. The monitored transition for DPN was mass to charge ratio (m/z) 339.0 → 167.0 for quantitation and 339.0 → 172.0 and 339.0 → 116.0 for confirmation. The linear range was 0.5 to 375 nanograms per milliliter (ng/mL). The average precision of DPN, represented by the relative standard deviation of the observed concentrations, was 7.2% and the average accuracy, represented by the relative error, was 5.8%. The recovery of DPN fortified at 3 different levels averaged 106% in rat liver and 101% in mouse liver. The established method was successfully used to determine DPN residue levels in Polynesian rats (Rattus exulans) and mice (Mus musculus) fed two different formulated baits containing DPN.

Data are provided as either a 'sample', 'calibration', or 'QC sample'. Where sample is used to designate something that has an unknown amount of diphacinone in it (can be a tissue extract, a reagent blank, or a diluent). Calibration is a standard that contains a known amount of diphacinone and is used to calibrate the mass spectrometer. QC is a sample with a known quantity of diphacinone in it that is used to assess the calibration for performance.

For complete details, see Goldade (2023).
Methodology_Citation:
Citation_Information:
Originator: Goldade, David A.
Originator: Siers, Shane R.
Originator: Hess, Steven C.
Originator: Sugihara, Robert T.
Originator: Riekena, Craig A.
Publication_Date: 2023
Title:
Determination of residue levels of rodenticide in rodent livers offered novel diphacinone baits by liquid chromatography-tandem mass spectrometry
Geospatial_Data_Presentation_Form: journal article
Series_Information:
Series_Name: PLOS One
Issue_Identification: 18(8): e0289261
Online_Linkage: https://doi.org/10.1371/journal.pone.0289261
Methodology_Citation:
Citation_Information:
Originator: Volker, Steve
Publication_Date: Unpublished material
Title:
NWRC Method 188A "Determination of Multiple Rodenticide Residues in Avian Liver By dSPE and LC/MS/MS"
Geospatial_Data_Presentation_Form: document
Other_Citation_Details:
Unpublished internal method. (For more information contact David Goldade, see contact information below.)
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Entity_and_Attribute_Information:
Overview_Description:
Entity_and_Attribute_Detail_Citation:
Below you will find a list and description of the files included in this data publication.

VARIABLE DESCRIPTION FILE (1)

1) \Data\_variable_descriptions.csv: Comma-separated values (CSV) file containing a list and description of variables found in all files. (A description of these variables is also provided in the metadata below.)

Columns include:

Filename = Name of data file
Variable = Name of variable
Units = Units (if applicable)
Description = Description of variable



DATA - tabular (10)

1) \Data\R20-006_Tabulated_Results.csv: CSV file containing a list of all the samples analyzed and the results for each sample.

Columns include:

Name = Unique sample name
Data File = The location (name of file) where raw data was saved at the time of acquisition
Type = Sample, Calibration, or QC sample
Acq. Date-Time = Date and time the sample was acquired (mm/dd/yyyy hh:mm)
Diphacinone RT = Retention time of the diphacinone peak in minutes
Diphacinone Resp. = Area response of the diphacinone peak in counts per second
Diphacinone MI = Indication of manual integration of the result (TRUE, FALSE)
Diphacinone Calc. Conc. = Calculated concentration of the diphacinone peak in nanograms per milliliter (ng/mL)
Diphacinone Final Conc. = Final concentration of the diphacinone peak in ng/mL
Height = Height response of the diphacinone peak (counts)
Noise = Height response in the specified noise region of the chromatogram (counts)
Qualifier (339.0 -> 172.0) Ratio = Area ratio of the qualifier transition to the quantifier transition
Qualifier (339.0 -> 172.0) MI = Indication of manual integration of the result (TRUE, FALSE)
Qualifier (339.0 -> 116.0) Ratio = Area ratio of the qualifier transition to the quantifier transition
Qualifier (339.0 -> 116.0) MI = Indication of manual integration of the result (TRUE, FALSE)
d4-Diphacinone (ISTD) RT = Retention time of the d4-diphacinone peak in minutes
d4-Diphacinone (ISTD) Resp. = Area response of the d4-diphacinone peak in counts per second


2-10) R20-006_[YYMMDD]_Part_[#]_QR_ISTD.xlsx: Microsoft Office Open XML spreadsheet files (9) containing all data for each of the 9 parts of this study. ([YYMMDD] = date of analysis and Part_[#] = Part_1 through Part_9). NOTE: The content of these worksheets is also provided as PDF files (\Data\PDF).

Each XLSX file contains the following worksheets:

Worksheet 1a: 'Summary - Sequence Table' = list of samples, quality control samples, and standards analyzed.

Columns include:

Data File = Name of the data file where raw data were saved at the time of acquisition
Sample Name = Name of the standard or sample
Sample Type = Sample, Calibration, or QC sample type
Position = Location of the sample vial at the time of injection
Volume = Volume of sample injected in microliters (µL)
Level = Name of the calibration level (L1-L8)
Acq Method File = Name of the method file used by the LC/MS/MS to aquire the raw data


Worksheet 1b: 'Summary - Quantification Results' = tabulated results of the instrumental analysis.

Columns include:

Sample Name = Name of the standard or sample
Compound = Name of the compound being evaluated
ISTD = Name of the internal standard
Sample Type = Sample, Calibration, or QC sample
RT = Retention time of the diphacinone peak in minutes
Response = Area response of the diphacinone peak in counts per second
ISTD RT = Retention time of the d4-diphacinone peak in minutes
ISTD Response = Area response of the d4-diphacinone peak in counts per second
Resp Ratio = Area ratio of the compound reponse to the internal standard response
Final Conc = Final concentration of the diphacinone peak in ng/mL
S/N = Ratio of peak hight to the reponse in the noise region
Accuracy = Percent match between the expected concentration and the final concentration


Worksheet 2a: 'Calibration' (above graph) = instrument calibration information.

Columns include:

Calibration STD = Name of the raw data file for each standard
Compound = Name of the compound being evaluated
Cal Type = Whether the data file is a calibration standard (CALIBRATION) or a QC sample (QC)
Level = Name of the calibration level (L1-L8)
Enabled = Status of inclusion in the calibration (enabled or not)
Response = Area response of the ISTD compound in counts per second
Exp Conc = Expected concentration of the ISTD for standards and QC samples in ng/mL
RF = Ratio of the area response of the ISTD to the expected concentration of the ISTD (response factor)


Worksheet 2b: 'Calibration' (below graph) = instrument calibration information.

Columns include:

Calibration STD = Name of the raw data file for each standard
Compound = Name of the compound being evaluated
Cal Type = Whether the data file is a calibration standard (CALIBRATION) or a QC sample (QC)
Level = Name of the calibration level (L1-L8)
Enabled = Status of inclusion in the calibration (enabled or not)
Response = Area response of the diphacinone in counts per second
Exp Conc = Expected concentration of the diphacinone standards and QC samples in ng/mL
RF = Ratio of the area ratio of the diphacinone to ISTD to the ratio of the expected concentration of the diphacinone to the ISTD (response factor)


Worksheets 3+ = worksheets named based on the standard, quality control sample, or study sample and include quantitation results, analysis information, and compound graphics.



DATA - PDF (18)
Data provided as XLSX files are also provided as Portable Document Format (PDF) files.

1-9) \Data\PDF\R20-006_[YYMMDD]_Part_[#]_QR_ISTD_SummaryCalibration.pdf: PDF files (9) containing the same content provided in the 'Summary' and 'Calibration' worksheets in \Data\XLSX\R20-006_[YYMMDD]_Part_[#]_QR_ISTD.xlsx. ([YYMMDD] = date of analysis and Part_[#] = Part_1 through Part_9)

10-18) \Data\PDF\R20-006_[YYMMDD]_Part_[#]_QR_ISTD_Results_AnalysisInfo: PDF files (9) containing the same content provided in the results and analysis information worksheets in \Data\XLSX\R20-006_[YYMMDD]_Part_[#]_QR_ISTD.xlsx. ([YYMMDD] = date of analysis and Part_[#] = Part_1 through Part_9)



SUPPLEMENTAL FILES (1)

1) \Supplements\DPN_MRM_220613_Method.pdf: PDF file containing a description of the operating conditions and parameters used to analyze the samples.
Entity_and_Attribute_Detail_Citation:
Goldade, David A.; Siers, Shane R.; Hess, Steven C.; Sugihara, Robert T.; Riekena, Craig A. 2023. Determination of residue levels of rodenticide in rodent livers offered novel diphacinone baits by liquid chromatography-tandem mass spectrometry. PLOS One. 18(8): e0289261. https://doi.org/10.1371/journal.pone.0289261
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Distribution_Information:
Distributor:
Contact_Information:
Contact_Organization_Primary:
Contact_Organization: USDA Forest Service, Research and Development
Contact_Position: Research Data Archivist
Contact_Address:
Address_Type: mailing and physical
Address: 240 West Prospect Road
City: Fort Collins
State_or_Province: CO
Postal_Code: 80526
Country: USA
Contact_Voice_Telephone: see Contact Instructions
Contact Instructions: This contact information was current as of March 2024. For current information see Contact Us page on: https://doi.org/10.2737/RDS.
Resource_Description: NWRC-RDS-2023-002
Distribution_Liability:
Metadata documents have been reviewed for accuracy and completeness. Unless otherwise stated, all data and related materials are considered to satisfy the quality standards relative to the purpose for which the data were collected. However, neither the author, the Archive, nor any part of the federal government can assure the reliability or suitability of these data for a particular purpose. The act of distribution shall not constitute any such warranty, and no responsibility is assumed for a user's application of these data or related materials.

The metadata, data, or related materials may be updated without notification. If a user believes errors are present in the metadata, data or related materials, please use the information in (1) Identification Information: Point of Contact, (2) Metadata Reference: Metadata Contact, or (3) Distribution Information: Distributor to notify the author or the Archive of the issues.
Standard_Order_Process:
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Microsoft Excel Open XML spreadsheet file
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Network_Resource_Name: https://doi.org/10.2737/NWRC-RDS-2023-002
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Format_Name: PDF
Format_Version_Number: see Format Specification
Format_Specification:
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Metadata_Reference_Information:
Metadata_Date: 20240301
Metadata_Contact:
Contact_Information:
Contact_Organization_Primary:
Contact_Organization: USDA, APHIS, Wildlife Service, National Wildlife Research Center
Contact_Person: David A. Goldade
Contact_Position: Supervisory Chemist
Contact_Address:
Address_Type: mailing and physical
Address: 4101 LaPorte Avenue
City: Fort Collins
State_or_Province: CO
Postal_Code: 80521
Country: USA
Contact_Voice_Telephone: 970-266-6080
Contact_Electronic_Mail_Address: david.a.goldade@usda.gov
Metadata_Standard_Name: FGDC Biological Data Profile of the Content Standard for Digital Geospatial Metadata
Metadata_Standard_Version: FGDC-STD-001.1-1999
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