A rapid imethod™ test for analysis of carbamate pesticides in beverages

A Rapid iMethod™ Test for the Analysis of Tetracyclines in Meat using Manual SPE iMethod™ Test for Tetracycline Antibiotics Version 1.0 for Cliquid® Software
Meat and other animal products need to be routinely monitored for veterinary drug residues that are used to fight disease and infection in animals, but are harmful to humans if present upon ingestion. However, with wide availability, variable legislation and variable animal husbandry practices from country-to-country, Strata™-X 33 µm polymeric SPE cartridge. This user-contributed high drug residue levels in produce continue to be an issue. iMethod™ test for Tetracyclines includes method documentation, Over-use and inappropriate use of antimicrobial drugs can lead MS and LC method files, processing method files and report to increased antimicrobial resistance, reducing the ability to fight templates, all deployed as a new iMethod test in your Cliquid® human infection. On top of this, exposure to such drugs can software. More in-depth sample preparation and instrument affect human reproduction, cause cancer and have a toxic effect. parameter information is included as part of the standard The following description outlines the instrument requirements operating procedure provided with the method, as are the and expected results obtainable from the iMethod™ test for the required analytical columns; solvents, standards and any quantification of five tetracycline antibiotics and metabolites supplies required for sample preparation are not included. when using an AB SCIEX 3200 QTRAP® LC/MS/MS instrument. The mobile phase consists of water with formic acid and Sample preparation is based on extraction with acidified acetonitrile with separation on Phenomenex Gemini C18 5µm methanol, followed by filtration, centrifugation, dilution with 4.6 x 50 mm HPLC column. An example chromatogram of the acidified water, and manual SPE clean-up on a Phenomenex separation achieved is shown below in figure 1. Figure 1. Example chromatogram for an injection of a 10 ppb standard, showing all the tetracyclines overlaid in one window (between 2.5 and
5.5 minutes).

Figure 2 illustrates the performance of the method for two Please note that the results presented were obtained using a transitions for all five analytes. In all cases the S/N is greater single instrument and single set of standards and samples, and than 7:1 for a 1 ppb injection on column. the results here may not be typical for all instruments. Prior to production use, the method should be fully validated with real samples. Variations in LC column properties, chemicals, environment, instrument performance and sample preparation procedures will impact performance, thus these results should be considered as informative rather than representative. Figure 2. Example Chromatograms for 1 ppb standards (signal-to-noise measured using PEAK:PEAK script).
The following two calibration curves are representative of the performance obtained on the instrument using the method described here. No internal standards were used in the analysis Figure 3. Calibration curve for chlortetracycline 1, standards 1 to 500 ppb (no internal standard used).
Figure 4. Calibration curve for methacycline 1, standards 1 to 500 ppb (no internal standard used).
System Requirements
Important Note
In order to run this method as outlined above, the following The purchase and use of certain of the chemicals listed above may require the end user to possess any necessary licenses, permits or approvals, if such are required in accordance with • An AB SCIEX 3200 QTRAP® LC/MS/MS System local laws and regulations. It is the responsibility of the end • Shimadzu XR HPLC system, or equivalent user to purchase these chemicals from a licensed supplier, if required in accordance with local laws and regulations. The suppliers and part numbers listed below are for illustrative purposes only and may or may not meet the aforementioned • A Phenomenex Gemini C18 5µm 4.6 x 50 mm HPLC local requirements. AB SCIEX is not responsible for user’s compliance with any statute or regulation, or for any permit or • Phenomenex Strata™-X 33 µm, Polymeric Sorbent approval required for user to implement any iMethod™ • Pipettes and standard laboratory glassware The iMethod™ test described above has been designed by Please note that the Phenomenex HPLC column is required AB SCIEX to provide the sample prep and instrument but not included with this iMethod™ test. This method can also parameters required to accelerate the adoption of this method be run on other HPLC systems, given that they are supported for routine testing. This method is provided for information for use by Cliquid® Software and the retention times are purposes only. The performance of this method is not updated to reflect the configuration used. guaranteed due to many different potential variations, including instrument performance, tuning, and maintenance, chemical Product Name
Part Number
variability and procedures used, technical experience, sample iMethod™ Test for Tetracyclines for Cliquid® matrices, and environmental conditions. It us up to the end user to make adjustments to this method to account for slight differences in equipment and/or materials from lab-to-lab as well as to determine and validate the performance of this method for a given instrument and sample type. Please note that a working knowledge of Analyst® Software may be For Research Use Only. Not for use in diagnostic procedures.
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Source: http://www.absciex.com/Documents/Downloads/Literature/iMethod%20Application%20for%20Tetracyclines%20in%20Meat_Manual%20SPE.pdf


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