High Sensitivity Analysis of Acrylamide in Potato Chips by LC/MS/MS with Modifed QuEChERS Sample Pre-treatment Procedure
Posters | 2014 | ShimadzuInstrumentation
Acrylamide is a thermal processing contaminant produced in carbohydrate rich foods at high temperatures via the Maillard reaction between asparagine and reducing sugars. Its potential neurotoxic and carcinogenic effects have elevated public health concerns and regulatory requirements for monitoring acrylamide levels in snacks and processed foods.
This study presents a high sensitivity LC/MS/MS approach for quantifying acrylamide in potato chips. The method combines a modified QuEChERS sample preparation for efficient defatting and cleanup with ultra fast UHPLC separation and triple quadrupole mass spectrometry, aiming for low detection limits, high recovery, and robust performance.
A 2 g potato chip sample was defatted with hexane, extracted with acetonitrile and QuEChERS salts, then water was removed by additional MgSO4. A dispersive SPE step removed organic acids. Extracts were evaporated under nitrogen and reconstituted in water. UHPLC separation employed a water–0.1% formic acid/methanol gradient at 0.2 mL/min and 40 ºC. Injection volume was 1 μL. MRM transitions for acrylamide (m/z 72.1>55.0, 72.1>27.1) and an acrylamide-d3 internal standard (m/z 75.1>58.0, 75.1>30.1) were optimized for sensitivity.
The method exhibited a linear response (R2>0.9999) over 1–500 ng/mL, with an intercept of 0.594. The blank potato chip extract contained 27.1 ng/mL acrylamide, corresponding to 135.5 ng/g. Limits of detection and quantification were estimated at <1 ng/mL and <3 ng/mL, respectively. Precision tests at 5 and 50 ng/mL yielded RSDs below 4%. Recovery efficiencies ranged from 104.7% to 112.0%, matrix effects between 84.6% and 96.5%, and overall process efficiency at 97.6%.
The method’s high sensitivity allows minimal injection volume, reducing system contamination when analyzing complex food matrices. Fast QuEChERS sample preparation and UHPLC–MS/MS analysis offer a streamlined workflow suitable for routine quality control and regulatory monitoring of acrylamide in processed foods.
Further developments may include integration of automated QuEChERS workflows, extension to other food matrices, and coupling with high-throughput screening platforms. Advanced mass spectrometry techniques could enable simultaneous determination of multiple processing contaminants in a single run.
A sensitive, accurate and robust LC/MS/MS method for acrylamide analysis in potato chips was established, featuring modified QuEChERS extraction, low detection limits, excellent linearity, precision, and recovery. It meets the demands of food safety monitoring and can be adapted to various processed products.
LC/MS, LC/MS/MS, LC/QQQ
IndustriesFood & Agriculture
ManufacturerShimadzu
Summary
Význam tématu
Acrylamide is a thermal processing contaminant produced in carbohydrate rich foods at high temperatures via the Maillard reaction between asparagine and reducing sugars. Its potential neurotoxic and carcinogenic effects have elevated public health concerns and regulatory requirements for monitoring acrylamide levels in snacks and processed foods.
Cíle a přehled studie / článku
This study presents a high sensitivity LC/MS/MS approach for quantifying acrylamide in potato chips. The method combines a modified QuEChERS sample preparation for efficient defatting and cleanup with ultra fast UHPLC separation and triple quadrupole mass spectrometry, aiming for low detection limits, high recovery, and robust performance.
Použitá instrumentace
- Shimadzu LCMS-8040 triple quadrupole mass spectrometer with UFMS technology
- Phenomenex Synergi Polar-RP 100A column (100 x 2.0 mm, 2.5 μm)
- RESTEK Q-sep QuEChERS extraction (Q100 packet) and d-SPE cleanup tubes (Q250)
- Electrospray ionization in positive MRM mode
Použitá metodika
A 2 g potato chip sample was defatted with hexane, extracted with acetonitrile and QuEChERS salts, then water was removed by additional MgSO4. A dispersive SPE step removed organic acids. Extracts were evaporated under nitrogen and reconstituted in water. UHPLC separation employed a water–0.1% formic acid/methanol gradient at 0.2 mL/min and 40 ºC. Injection volume was 1 μL. MRM transitions for acrylamide (m/z 72.1>55.0, 72.1>27.1) and an acrylamide-d3 internal standard (m/z 75.1>58.0, 75.1>30.1) were optimized for sensitivity.
Hlavní výsledky a diskuse
The method exhibited a linear response (R2>0.9999) over 1–500 ng/mL, with an intercept of 0.594. The blank potato chip extract contained 27.1 ng/mL acrylamide, corresponding to 135.5 ng/g. Limits of detection and quantification were estimated at <1 ng/mL and <3 ng/mL, respectively. Precision tests at 5 and 50 ng/mL yielded RSDs below 4%. Recovery efficiencies ranged from 104.7% to 112.0%, matrix effects between 84.6% and 96.5%, and overall process efficiency at 97.6%.
Přínosy a praktické využití metody
The method’s high sensitivity allows minimal injection volume, reducing system contamination when analyzing complex food matrices. Fast QuEChERS sample preparation and UHPLC–MS/MS analysis offer a streamlined workflow suitable for routine quality control and regulatory monitoring of acrylamide in processed foods.
Budoucí trendy a možnosti využití
Further developments may include integration of automated QuEChERS workflows, extension to other food matrices, and coupling with high-throughput screening platforms. Advanced mass spectrometry techniques could enable simultaneous determination of multiple processing contaminants in a single run.
Závěr
A sensitive, accurate and robust LC/MS/MS method for acrylamide analysis in potato chips was established, featuring modified QuEChERS extraction, low detection limits, excellent linearity, precision, and recovery. It meets the demands of food safety monitoring and can be adapted to various processed products.
Reference
- Swedish National Food Administration Information about acrylamide in food April 2002
- Mottram DS Wedzicha BL Nature 419 2002 448-449
- Ahn JS Castle JB Clarke DB Lloyd AS Philo MR Speck DR Food Addit Contam 19 2002 1116-1124
- Mastovska K Lehotary SJ J Agric Food Chem 54 2006 7001-7998
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