58 Food & Beverage Analysis
When MS source maintenance is not required, the collared nut in combination with the column installation tool allows installation of the column into the MS without opening the side door. Gold-plated fl exible metal ferrules are inert and provide exceptionally reliable sealing. They prevent formation of microleaks and help maintain high sensitivity of the GC/TQ.
The system’s air/water check, or autotune report, can signal the presence of leaks. However, this approach does not help to identify the source of the leak. Additionally, it may miss microleaks like those that may be present at user connections.
Pentachloronitrobenzene presents a challenge for LC/MS analysis, so GC/MS analysis is the technique of choice.
Optimised injection with the temperature- programmable multimode inlet
Effi ciently volatilising the sample in the GC inlet is an essential component of a successful GC/MS analysis. Some pesticides, such as captafol, captan, dicofol, folpet, and deltamethrin, are known to suffer thermal degradation during injection. Starting the injection at lower temperature of 60°C and ramping up to 280°C allows for volatilising all the target analytes while maintaining their chemical integrity upon introduction to the GC column. Moreover, the ability to program the inlet temperature allows heating up the inlet further to 310°C during the post run while backfl ushing. This heating enables the system to bakeout any matrix residue that may remain in the inlet. The combination of temperature-programmable injection with a ultra-inert 2 mm dimpled liner resulted in high sensitivity, even for challenging pesticides like deltamethrin in a complex walnut matrix. Figure 5A shows the response of deltamethrin, a pesticide with an established MRL in walnuts, at 0.5 ppb.
Figure 5B shows the chromatograms for a selective multiple reaction monitoring transition for pentachloronitrobenzene, a commonly analysed pesticide, in a walnut extract. Pentachloronitrobenzene has established MRLs in many vegetables and fruits, peanuts, and soybean seeds that vary from 20 ppb to 1 ppm [4]. Pentachloronitrobenzene presents a challenge for LC/MS analysis, so GC/MS analysis is the technique of choice.
Multi-class, multi-residue pesticide GC/MS/MS testing allows for routine monitoring, enabling high throughput, sensitive detection levels, and rapid quantitative analysis for hundreds of pesticides in a single sample. Implementing these fi ve key practices when analysing pesticides in challenging food matrices including spinach, walnut and cayenne pepper, allows for excellent calibration performance for the resulting method, over a wide dynamic range up to over four orders of magnitude. Consider implementing these measures to reduce matrix interferences with target analytes and extend your instrument’s maintenance-free operation time.
References 1.
https://www.who.int/news-room/fact-sheets/detail/pesticide-residues-in-food
2. Setting Tolerances for Pesticide Residues in Foods, US EPA
https://www.epa.gov/pesticide-tolerances/ setting-tolerances-pesticide-residues-foods. Accessed on December 5, 2022.
Figure 5. MRM chromatograms for deltamethrin (A) and pentachloronitrobenzene (B) at 0.5 ppb in walnut extract analysed with the 7000E and 7010 GC/TQ
With the recent advancements in GC/MS software, the source of the leak can be identifi ed through monitoring user-specifi c ions and plotting corresponding chromatograms.
Multi-class, multi-residue pesticide GC/MS/MS testing allows for routine monitoring, enabling high throughput, sensitive detection levels, and rapid quantitative analysis for hundreds of pesticides in a single sample. Implementing these five key practices when analysing pesticides in challenging food matrices including spinach, walnut and cayenne pepper, allows for excellent calibration performance for the resulting method, over a wide dynamic range up to over four orders of magnitude. Consider implementing these measures to reduce matrix interferences with target analytes and extend your instrument's maintenance-free operation time.
DE90315046 Flow Sensing Challenges in Food and Beverage Production
Titan Enterprises offers a range of high-performance flowmeters in food grade materials where both food hygiene and precision flow measurement are required. “The physical properties of the liquids themselves lend additional complexities to the choice of flow measuring equipment,” says Neil Hannay, Senior Development Engineer at Titan Enterprises. “Consideration of whether the liquid is viscous, volatile, corrosive, flammable, or contaminated with particles, for example, or needs to be maintained at a high temperature, are key factors in deciding a suitable flow meter.”
Flow monitoring of high viscosity liquids, such as cooking oils, sauces and syrups (e.g. syrup injections in beverage lines) require devices such as Titan’s oval gear flowmeters, which provide highly accurate flow measurement. Unlike other flowmeters, measurement accuracy of oval gear flowmeters improves as the liquid viscosity increases, from a nominal 1% to around 0.1% of flow rate at higher viscosities.
Whereas for low viscosity liquids such as water, beer, wine and spirits, Titan’s NSF-approved 800-series and beverage flowmeters provide a low-cost drink dispensing solution. Designed to give high performance over 6 flow ranges from 0.05 to 15 l/min, these devices have totally non-metallic NSF-approved wetted components making them ideally suited for applications where both food hygiene and precision flow measurement are required.
In processes where ingredients need to be maintained at high temperatures – chocolate for example – a flowmeter designed for applications requiring precise flow measurement at elevated temperatures would be needed. Capable of operating up to 110°C, Titan’s inline non-invasive Atrato® ultrasonic flowmeter is largely immune from viscosity and offers excellent turndown and repeatability.
Titan Enterprises offers a range of oval gear flowmeters in food grade materials for viscous products such as sauces, oils and syrups, as well as NSF-approved mini-turbine flowmeters for drink dispensing. As an experienced OEM supplier, Titan develop customised flow meters for specific customer applications within the food and beverage industry.
More information online:
ilmt.co/PL/Z469 and
ilmt.co/PL/Vod3 59555pr@reply-direct.com
Figure 5. MRM chromatograms for deltamethrin (A) and pentachloronitrobenzene (B) at 0.5 ppb in walnut extract analysed with the 7000E and 7010 GC/TQ
3. Index to Pesticide Chemical Names, Part 180 Tolerance Information, and Food and Feed Commodities (by Commodity), US EPA. December 12, 2012.
https://www.epa.gov/sites/default/fi les/2015-01/documents/ tolerances-commodity.pdf. Accessed on December 5, 2022.
4. 40 CFR § 180.291 - Pentachloronitrobenzene; Tolerance for Residues.
https://www.law.cornell.edu/cfr/ text/40/180.291. Accessed on December 5, 2022.
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New Profi ciency Test for Fish Analysis
BIPEA has launched a new Proficiency Testing Schemes (PTS 20G) which allows testing laboratories to evaluate their analytical performances by analysing fish samples. For this test, laboratories will be able to analyse a 600g frozen fish sample according to their usual methods. This PT offers the following parameters: Caloric value (moisture, ashes, water activity, pH, proteins, cholesterol, energy values…), Freshness (total volatile nitrogen (TVB-N), trimethylamine (TMA), Mineral (Calcium, Copper, Iron, Manganese, Magnesium…), Vitamins (Tocopherols, B1, B2, PP…), Fatty acid profile, Premi®Test.
To learn more about the “PTS 20G - Fish and fishery products”, as well as the full range of proficiency tests, please feel free to contact BIPEA. More information online:
ilmt.co/PL/Yvno
59492pr@reply-direct.com
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