Home

Agilent 320-MS Qualifier Assessment Ion Ratio Stability Manual

1. 64 7 1047 Ea 2 146 148 150 152 14 minutes v Add Scan Function Channels a lt 313 0241 0 33 0 31 gt a 5 Delete 5 Update Ratios From Data File Current Ret Time min 15 015 PEA Nest Close Restore Figure 1 320 MS Method Editor Summary of Experiment Aflatoxins B1 and B2 were obtained from Sigma Aldrich The LC MS MS was done on the 320 MS The ion ratios were estimated by the software The ion ratios for the above compounds and their respective tolerance levels as per EU criteria are given in Table 2 Quan lon Qualifier lon Tolerance Target analyte Transition Transitions lon ratio EU Criteria Aflatoxin B1 3135285 3135241 84 7 20 Aflatoxin B2 315287 315 259 18 0 30 Table 2 lon ratios for Aflatoxins B1 and B2 on the 320 MS and their respective tolerance levels as per EU criteria Technologies For more information go to www agilent com chem NOTICE This document contains references to Varian Please note that Varian Inc is now part of Agilent 2 Agilent Technologies The overlaid chromatograms of the qualifier and quantifier ions give an idea of the qualifier assessment Figure 2 Aflatoxin B1 313 0 gt 285 0 22 0V 313 0 gt 241 0 33 0V Sour Aflatoxin B2 315 0 gt 287 0 21 5V 315 0 gt 259 0 1 0 0V Figure 2 Qualifier ion assessments for Aflatoxins B1 and B2 on the 320 MS The above compounds were spiked
2. 20 79 10 5 6 18 00 30 17 70 0 3 350 84 70 20 78 20 6 5 18 00 30 17 50 0 5 35 84 70 20 79 20 5 5 18 00 30 17 30 0 7 35 84 70 20 79 40 5 3 18 00 30 17 90 0 1 35 84 70 20 79 00 5 7 18 00 30 17 30 0 7 3 5 84 70 20 79 60 5 1 18 00 30 17 80 0 2 3 5 84 70 20 79 60 5 1 18 00 30 17 40 0 6 3 5 84 70 20 78 90 5 7 18 00 30 17 50 0 5 0 35 84 70 20 77 00 7 7 18 00 30 18 60 0 6 0 35 84 70 20 73 10 11 6 18 00 30 19 60 1 6 0 35 84 70 20 74 40 10 3 18 00 30 17 00 1 0 Mean 7 15 0 61 SD 29 0 3 Table 3 Observed ion ratio tolerances for Aflatoxins B1 and B2 over four orders of magnitude on the 320 MS triple quadrupole system Aflatoxin B1 Aflatoxin B2 Specified lon ratio Actual Qvserved loniratio Specified lon ratio Actual lon ratio Observed loni ratio lon ratio Tolerance Tolerance 84 70 77 10 7 60 18 00 18 30 0 30 84 70 77 70 7 00 18 00 18 00 0 84 70 78 30 6 40 18 00 18 10 0 10 84 70 77 70 7 00 18 00 18 10 0 10 84 70 78 10 6 60 18 00 18 20 0 20 84 70 77 40 7 30 18 00 18 10 0 10 84 70 77 10 7 60 18 00 18 50 0 50 84 70 77 30 7 30 18 00 18 00 0 84 70 77 20 7 50 18 00 18 30 0 30 Mean 7 14 0 2 SD 0 43 0 2 Table 4 lon ratio stability in wheat beer Page 2 As seen from the table the observed ion ratio tolerances for both the compounds in wheat beer were well below the permitted tolerance l
3. Varian 320 MS O _ zz Qualifier Assessment and lon Ratio Stability Advantage Statement Varian s 320 MS triple quadrupole system meets the quality guidelines for qualifier assessment and ion ratio stability set by the European Union for the detection and analysis of toxic compounds The toxicological quality guidelines set by the European Union for the detection of toxins and drugs by LC MS MS systems recommends the use of at least one qualifier ion for the confirmation of target analytes A minimum of at least one ion ratio must be measured and all the measured ion ratios must meet the criteria for the allowable tolerances The allowable tolerances mainly depend on the relative intensity of the qualifier ion with respect to the base peak quantifier ion Table 1 gives the maximum permitted tolerance for relative ion intensities for LC MS MS set by European Commission Council Directive 96 23 EC SANCO 1805 2000 1 Relative Intensity of base peak Maximum permitted tolerance for relative ion intensity with LC MS MS gt 50 20 gt 20 50 25 gt 10 20 30 lt 10 50 Table 1 Maximum permitted tolerances for relative ion intensities using LC MS MS set by European Union European Commission Council Directive 96 23 EC SANC0 1805 2000 The applicability of the above criteria for LC MS MS on Varian s 320 MS triple quadrupole system was evaluated using the carcinogenic mycotoxins Aflatoxins B1 and B2 F
4. evels set by European Union The 320 MS provides e Excellent ion ratio stability across a wide calibration range e The solution to meet and or exceed the demanding EU ion ratio tolerance guidelines e Highly reproducible analytical results in heavy matrices e A sensitive robust and rugged LC MS MS methodology for the determination of mycotoxins NOTICE This document contains references to Varian Please note that Varian Inc is now part of Agilent Technologies For more information go to www agilent com chem EE Agilent Technologies European Commission Decision laying down performance criteria for the analytical methods to be used for detecting certain substances and residues thereof in live animals and animal products according to Council Directive 96 23 EC SANCO 1805 2000 Rapid Quantitative Analysis of Multiple Mycotoxins by Liquid Chromatography Tandem Mass Spectrometry Rudrabhatla et al American Lab April 2007 22 25 Varian Inc www varianince com North America 800 926 3000 925 939 2400 Europe The Netherlands 31 118 67 1000 Asia Pacific Australia 613 9560 7133 Latin America Brazil 11 3845 0444 Other sales offices and dealers throughout the world GC LC MSe AA ICP ICP MS e UV Vis NIR FT IR Raman e Fluorescence Dissolution e NMR MRI Consumables Data Systems SI 0626 05 07 Printed in U S A
5. in buffer at concentrations ranging from 0 35 ppb to 350 ppb i e over four orders of magnitude They were run in triplicate on the 320 MS The ion ratio tolerance was assessed over the entire range The specified ion ratios actual ion ratios and the deviation from the specified ion ratios are given in Table 3 As seen from Table 3 the observed ion ratio tolerance for Aflatoxin B1 ranged from 5 1 to 11 6 The average tolerance observed was 7 15 This is far less than the tolerance level of 20 set by the European Union For Aflatoxin B2 the observed ion ratio tolerance was found to be around 0 6 far below the required 30 Spike concentration had very little effect on the ion ratio tolerance indicating the exceptional stability and linearity of the 320 MS for the analysis of toxic compounds The ion ratio stability was also tested in a complex matrix Wheat beer was spiked with 40 ppb each of Aflatoxins B1 and B2 and purified using a solid phase extraction cartridge Nine replicates were run on the 320 MS The ion ratio stability was assessed Table 4 AflatoxinB1 Aflatoxin B2 Observed lon Observed lon Concentration Specified lon Tolerance levels ratio Specified lon Tolerance levels ratio in ppb ratio set by EU Actual lon ratio Tolerance ratio set by EU Actual lon ratio Tolerance 350 84 70 20 79 10 5 6 18 00 30 17 50 0 5 350 84 70
6. or more information about the analytical methodology see Reference 2 Qualifier Assessment using the 320 MS Method Editor The quan ions dialog box of the 320 MS method editor allows the user to specify the quantifier and qualifier ions from a reference spectrum Figure 1 The product ion with the highest intensity from a Multiple Reaction Monitoring MRM experiment is chosen by the user as the quantifier ion and the remaining ions from the reference spectrum are loaded or added as qualifiers to the qualifiers table The software integrates the peak areas and automatically enters the ratio of the qualifier ion to the quan ion in the ratio field with a default 20 tolerance level The user can increase or decrease the tolerance level manually if needed Compound Attributes Quanlons Calculations Integration Identification Reef Spectum 45 015 AfletoxinB1 285 0 c 1 2 Linear Ignor 5 0 30 w 12 0 S 0 40 Near 285 0 241 0 MCountsd 4 WB_BEM med 9 2 2006 xms d Search 15 019 min Scan 2953 0 a B ee 10 04 4 5 04 P 079e iddi E J J 0 0 754 nile Match Reference el 50 3 15 051 min Scan 2953 d 2 kcountg 241 00 285 0 2 54 4 0 504 995 99974 0 04 be T T 4 0 005 7 T 7 7 R match 98 F Mateh 006 Miz Qualifiers Absolute Quan lon Pts Integration Report As Failed Quan lons lon Z Ratio Uncert Low High Load 1 241 0 84 7 20 0

Agilent 320-MS Qualifier Assessment Ion Ratio Stability Manual

Contents

Download Pdf Manuals

Related Search

Related Contents