Page 23 - Food&Beverages Solution Palm Oil

Gas Chromatograph Triple Quadrupole

Mass Spectrometer (GC/MS/MS) High Performance Liquid Chromatograph (HPLC)

Triglycerides

The Evaporative Light-Scattering Detector (ELSD-LT) is a universal detector for HPLC. The ELSD-LT can remove the mobile phase through
evaporation and then make a light scattering measurement of the dried analyte particle.

In principle, the ELSD-LT can detect all sample compounds that are not volatile ones, so it is ideally suited for those that have low
absorbance and are difficult to detect using a UV detector such as sugars, fats and surfactants. Furthermore, it can be used for a
wide range of applications, since it can be used with gradient elution for optimized separations and reduced run times, which is not
possible with a Refractive Index Detector (RID). This example introduces an analysis triglycerides (triacylglycerols) contained in
Representative MRM chromatogram where 3-MCPD-d5, 3-MCPD, 2-MCPD, glycidol-d5 and glycidol were eluted at 18.4 min, 18.6 min, 19.6 min, 21.6 min and 21.7 min, respectively. cooking oil using the ELSD-LT.
Reference: Determination of Fatty Acid Esters of 2- and 3-Monochloro-1,2-propanediol (MCPD) and Glycidol in Edible Oil Using GC/Triple Quadrupole MS
Polycyclic Aromatic Hydrocarbons (PAHs) Analytical Conditions

In recent years, there has been a trend toward viewing high concentrations of polycyclic aromatic hydrocarbons (PAHs) in foods Column :Shim-pack VP-ODS (250 mmL. × 4.6 mmI.D.)
(particularly smoked products) as a problem. In 2009, the Codex Alimentarius Commission issued standards for reducing the PAH Mobile phase :Acetonitrile/ Acetone=3 / 7(v/v)
Flow rate
:1.0 mL/min
contamination level in smoked and directly dried foods. In addition, Europe, Canada, South Korea, China, and others established food Column temperature :30°C
standards for benzo[a]pyrene. Shown here is an example of GC-MS/MS analysis of PAHs in "katsuobushi" (dried, smoked, and Detection :ELSD-LT
fermented skipjack tuna, which is very popular in Japanese cuisine). Temperature :35°C
GAIN :5
Analytical Conditions (Left) GC-MS (SIM) (Right) GC-MS/MS (MRM) Nebulizer gas :Air
Benzo[a] Gas pressure :350 KPa
GC-MS :GCMS-TQ8040 pyrene
Column :Rxi-PAH (60 m long, 0.25 mm I.D., df = 0.1 µm) (RESTEK, P/N: 49317)
Glass insert :Splitless insert with wool (Shimadzu, P/N: 221-48876-03)
[GC] [MS]
Injection volume :2 µL Interface temperature :330ºC
Injection unit temperature :330ºC Ion source temperature :230ºC Indeno
Column oven temperature :180ºC (2 min) (5ºC /min) Measurement mode :MRM [1,2,3-cd]
260ºC (15ºC/min) 350ºC (12 min) Loop time :0.3 sec pyrene
Carrier gas control :Constant linear velocity (40.0 cm/sec)
Injection mode :Splitless
Sampling time :2 min
Carrier gas :Helium SIM and MRM Chromatograms of PAHs in Katsuobushi Extract

Reference: Application News MS109 - Analysis of Polycyclic Aromatic Hydrocarbons (PAHs) in Foods by GC-MS/MS
Shimadzu Gas Chromatograph Triple Quadrupole Mass Spectrometer Product Lineup

Model Features
· GCMS-TQ8040 with MRM Optimization Tool seamlessly selects and optimizes MRM transitions for multiple
compounds in a single sequence
· Smart Database series provides fully automated method development at the touch of a button
· Smart MRM method creation protocol automatically sets the optimum dwell and loop times for each method to maximize sensitivity
· Flexible MS Events prevent losing compounds in the presence of a complex matrix
· Scan/MRM analysis mode simultaneously acquires accurate library-searchable mass spectra and low-level MRM quantitation in a single analysis
GCMS-TQ8040 · Automatic Adjustment of Retention Times (AART) with > 99.9% accuracy means no need to adjust flow rates or update RTs manually

· Better amplification performance that maximizes use of Off-Axis Ion Optics made possible by new long-life detector
· Contamination-resistant ion source coupled with a new long life-detector ensures reliable analysis with less maintenance requirements
· Large-capacity turbomolecular pump with improved exhaust efficiency allows for higher sensitivity and stability Chromatogram of a Standard Mixture of Triglycerides
· Smart MRM technologies coupled with the use of LabSolutions Insight improve ease of method creation and data review (upper: ELSD-LT, lower: RID)
· High-speed scan and data acquisition using Advance Scanning Speed Protocol (AASP) to achieve speeds up to 20,000 µ/sec across all masses
· Ecology mode reduces costs associated with power and carrier gas consumption
GCMS-TQ8050 · Various configurations enable optimal performance for specific analytical needs
Reference: Application News No. L290A Application of Evaporative Light-Scattering Detector “ELSD-LT” (Part1) Analysis of Triglycerides in Cooking Oil

Solutions for Palm Oil Analysis Application Notebook
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