Method for Determining 3 Preservatives in Food Using the Anyeep TQ9120 Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry System
This study utilized the Anyeep TQ9120 ultra-high-performance liquid chromatography-tandem mass spectrometry system from Anyeep to develop a method for simultaneously detecting 3 preservatives in food. The method demonstrated excellent linearity, with limits of detection and quantification meeting relevant regulatory standards. Using this method and equipment enables accurate detection and quantification of preservatives.
Baked goods are nutrient-rich matrices with high sugar and moisture content, including bread, cakes, pastries, mooncakes, and pastry fillings. These products are prone to microbial growth and spoilage during storage and distribution. Benzoic acid, sorbic acid, and dehydroacetic acid are common preservatives used in the baking industry; however, excessive use, use beyond approved scopes, or combined use can pose food safety risks. Consequently, they are key targets for market inspections. Testing samples include pre-packaged finished products, bulk items, semi-finished baked goods, and fillings.
The industry's primary authoritative standard for regulating this preservative is GB 2760-2024 "National Food Safety Standard—Use of Food Additives," which explicitly prohibits the addition of benzoic acid to baked goods and sets compliance limits for the maximum usage of sorbic acid and dehydroacetic acid. Routine detection methods typically employ liquid chromatography per GB 5009.28-2016 and GB 5009.121-2016, enabling precise identification of illegal additions and exceedances. This provides an effective technical basis for quality control and market regulation of baked goods. The method described herein references existing literature and utilizes the external standard method for quantification.
Instruments and Reagents
AnyeepTQ9120 Ultra-High Performance Liquid Chromatography-Tandem Mass SpectrometrySystem
Methanol(Mass spec only,)Shanghai ANPEL）
Ammonium acetate (HPLC grade,Shanghai ANPEL）
Glacial acetic acid (Pure analysisShanghai ANPEL）
n-Hexane (Chromatographic gradeShanghai ANPEL）
Ethanol (Chromatographic gradeShanghai ANPEL）
Potassium ferrocyanide (Pure analysisShanghai ANPEL）
Zinc acetate (Pure analysisShanghai ANPEL）
Liquid Chromatography Conditions
Mobile PhaseA: 1 mM ammonium acetate-water
Mobile Phase B: Methanol
Chromatography column: CNW Athena UHPLC C18 Column 1.8μm, 2.1×100 mm
Column Temperature：40 ℃
Flow rate: 0.3 mL/min
Injection volume：5 μL
Mass Spectrometry Conditions
Ionization Source： Electrospray Ionization Source (ESI)-）
Source Temperature： 550℃
Spray Voltage： 4500V
air curtain： 45 psi
Mist gas： 60 psi
Auxiliary Gas： 60 psi
Crash： 7
Scan Mode：MRM
Sample Processing
Sample ProcessingWeigh 2 g of the sample (accurate to ±0.01 g). Add 10 mL n-hexane, vortex for 1 min, and ultrasonicate for 10 min. Centrifuge at 4000 r/min for 5 min, then discard the n-hexane. To the residue, add 2 mL ethanol, 2 mL potassium ferrocyanide solution, and 2 mL zinc acetate solution. Vortex to mix, then add 15 mL ultrapure water. Ultrasonicate for 30 min, centrifuge at 12000 r/min for 3 min, and transfer the supernatant to a 25 mL volumetric flask. Dilute to the mark with water. Transfer 5 mL of the sample solution onto an HLB solid-phase extraction column preconditioned with methanol and water. Wash the HLB column with 5 mL methanol and collect all eluate. Nitrogen blow at 50 °C until nearly dry. Dissolve the residue in 1 mL of 50% methanol-water solution and pass through 0.22.μFilter through m membrane.Collect the filtrate for analysis.
Standard Curve PreparationAccurately pipette an appropriate amount of the mixed standard working solution and dilute it with blank matrix to 2.μg/L5μg/L、10μg/L20μg/L50μg/L100μg/L200μg/L500μg/L、1000μg/L series standard solutions for determination by liquid chromatography-tandem mass spectrometry (LC-MS/MS).
Summary
This study established a detection method for 3 preservatives using the Anyeep TQ9120 ultra-high-performance liquid chromatography-tandem mass spectrometry system. Results demonstrate that this method offers excellent sensitivity, stability, and linear range, making it suitable for routine preservative analysis.