#foodsafety #enviromental
Automated determination of glyphosate, AMPA and glufosinate in food
by online ligand exchange SPE-LC-MS/MS
This workstation by Axel Semrau® has been developed to determine glyphosate, glufosinate, and AMPA in complex matrices, for example, foodstuff.
The CHRONECT Symbiosis | Glyphosate consists of an XYZ robot with a centrifuge, vortexer, and agitator, an online SPE unit with prepared methods, and the specialized cartridges CHROSPE Glyphosate. Utilization of standard SPE cartridges for simple matrices, e.g., C8 or C18 phases, is possible.
NOTE – CHRONECT Workstation Glyphosate will be delivered with ready-for-use methods for different matrices.
ABOUT GLYPHOSATE
Glyphosate is one of the most widely used active chemicals in pesticides to prevent undesirable plant growth around planted crops or to eradicate plants or parts of plants. These chemicals are commonly referred to as weedkillers or herbicides.
Glyphosate works by preventing plants from making certain proteins that are necessary for growth.
When used precisely and according to label instructions, it helps to keep weeds from competing with crops for water, sunlight, and nutrients.
Glyphosate helps farmers and homeowners control weeds in many different kinds of plantings, including a wide variety of fruit, vegetable, and other food crops.
The main metabolite of glyphosate: AMPA (Aminomethylphosphonic Acid)
Glufosinate — Structurally similar compound
SAFETY INFORMATION
Public discussions about toxicity and carcinogenicity
Worldwide discussions about possible cancerogenic and/or mutagenic effects.
The European Food Safety Authority (EFSA) has stated that glyphosate is:
“unlikely to pose a carcinogenic hazard to humans.”
New Zealand’s Environmental Protection Agency concluded in a report issued in August 2016 that glyphosate is:
“unlikely to be carcinogenic.”
In a joint report issued in 2016, the U.N.’s Food and Agriculture Organization (FAO) and World Health Organization (WHO) said glyphosate is:
“unlikely to pose a carcinogenic risk to humans.”
exposed to it through dietary exposure.
ANALYSIS OF GLYPHOSATE
WORKFLOW
CHEMICAL ANALYSIS OF
GLYPHOSATE, AMPA & GLUFOSINATE
Using online SPE-LC-MS/MS, glyphosate is concentrated on specific cartridges. Combined with a Sciex Triple Quad 5500 system, the determination limit for wheat, black tea & sunflower seeds, difficult matrices, are below 3 µg/kg. An excellent recovery between 86 and 96 % and a repeatability of ~ 10 % were measured for the detection of glyphosate, AMPA and glufosinate for each matrix. This proves that the method is very reliable.
Analysis
Spiking at LOQ 3 µg/kg (n=6)
Requirements:
- Signal-to-noise ratio ≥10:1
- Spiking at 10, 50 and 100 µg/kg (n=3 each)
- Repeatability RSDr ≤20%
- Trueness 70-120%
- Retention time deviation between samples and standards: ≤0.1 min
- Ion ratio deviation between samples and standards: ≤30 %
- Linearity
Wheat
Wheat spiked with 3 µg/kg
Glyphosate MRM 390 → 168
AMPA MRM 332 → 110
Glufosinate MRM 402 → 180
Black Tea
Tea spiked with 3 µg/kg
Glyphosate MRM 390 → 168
AMPA MRM 332 → 110
Glufosinate MRM 402 → 180
Sunflower Seeds
Sunflower seeds spiked with 3 µg/kg
Glyphosate MRM 390 → 168
AMPA MRM 332 → 110
Glufosinate MRM 402 → 180
VALIDATION
Analysis of Glyphosate
complex matrices – basic validation
Analysis of AMPA
complex matrices – basic validation
Analysis of Glyphosinate
complex matrices – basic validation
CONCLUSIONS – OUTLOOK
The presented method allows a time-efficient sensitive detection and quantification of glyphosate, AMPA and glufosinate in complex food matrices. The manual effort is minimized by applying online SPE. The ligand exchange SPE material reduces matrix effects to a minimum. Signal to noise-ratios at 3 µg/kg are satisfactory, even for complex matrices.
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