کد مقاله | کد نشریه | سال انتشار | مقاله انگلیسی | نسخه تمام متن |
---|---|---|---|---|
1164936 | 1491052 | 2013 | 9 صفحه PDF | دانلود رایگان |
• The quadrupole in Q Exactive acts as a powerful filter to reduce ion suppression.
• Reducing mass range using quadrupole in targeted modes increases the S/N ratio.
• Targeted SIM data dependent scan modes are the most suitable for residue analysis.
• A HRMS confirmatory method for synthetic hormones in urine has been developed.
• The Q Exactive provides similar sensitivity and enhanced selectivity compared to QqQ.
Sensitive and unequivocal determination of analytes/contaminants in complex matrices is a challenge in the field of food safety control. In this study, various acquisition modes (Full MS/AIF, Full MS + tMS/MS, Full MS/dd MS/MS and tSIM/ddMS/MS) and parameters of a quadrupole–orbitrap hybrid mass spectrometer (Q Exactive) were studied in detail. One of the main conclusions has been that, reducing the scan range for Full MS (using the quadrupole) and targeted modes give higher signal-to-noise (S/N) ratios and thereby better detection limits for analytes in matrix. The use of Q Exactive in a complex case, for the confirmatory analysis of hormones in animal urine is presented. A targeted SIM data dependent MS/MS (tSIM/ddMS/MS) acquisition method for determination of eight synthetic hormones (trenbolone, 17α ethinylestradiol, zeranol, stanozolol, dienestrol, diethylstilbestrol, hexestrol, taleranol) and a naturally occurring hormone (zearalenone) in animal urine were optimized to have sensitive precursors from targeted SIM mode and trigger MS/MS scans over the entire chromatograph peak. The method was validated according to EC/657/2002. CCα (decision limit) for the analytes ranged between 0.11 μg L−1 and 0.69 μg L−1 and CCβ (detection capability) ranged between 0.29 μg L−1 and 0.90 μg L−1.
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Journal: Analytica Chimica Acta - Volume 780, 30 May 2013, Pages 65–73