EconoTrace - a pretreatment solution for nitrosamines in drinking water

First, the preface

It is well known that nitrosamines are a class of highly carcinogenic compounds that are widely found in our food, consumer products and drinking water. Especially in recent years, people have found the presence of nitrosamines in drinking water, sewage treated water bodies and water bodies directly contaminated by industrial sources. Because nitrosamine disinfection by-products are low in water (usually <1 ng/L) and most of the compounds are water soluble, it is difficult to analyze them, whether it is analytical methods, formation mechanisms or control methods. There are still many blind spots in the research, and the variety of variability and the limitations of existing science and technology, the detection of nitrosamines is very challenging.

At present, there is no uniform standard for the analysis methods of nitrosamines in drinking water in China. Therefore, this method refers to the sample pretreatment method of US EPA Method521, using FMS's Econotrace synchronous solid phase extraction system for nitrous oxide in drinking water. The amine is enriched and extracted, and is detected by a nitrosamine-specific detector. The final recovery rate is good, and it is suitable for the detection of nitrosamines in drinking water. In this method, FMS's EconoTrace synchronous solid phase extraction system is used in conjunction with the SuperVap nitrogen blowing concentration system to realize the whole process of solid phase extraction-concentration, simplifying the solid phase extraction step, eliminating many manual operations and greatly improving the efficiency. , reducing human error.

Second, experimental reagents and consumables

1. Activated carbon solid phase extraction column, 2g

2. Dichloromethane reagent (agricultural residue level)

3. Methanol reagent (agricultural residue level)

4. Deionized water reagent (chromatographic grade)

5. Sodium thiosulfate extraction column, 2g

6. Laboratory nitrosamine solution sample (US-113N)

7. d6 nitrosodimethylamine mixture sample (IST-760)

8. d14 dipropyl nitrosamine mixture sample (IST-770)

Third, the experimental instrument

FMS EconoTrace Synchronous Solid Phase Extraction System

FMS SuperVap Nitrogen Blowing Concentration System

FMS one-step sample concentrator

Nitrosamine detector

Fourth, the setting procedure of EconoTrace synchronous solid phase extraction system

1. Activate the solid phase extraction column with 5 ml of dichloromethane

2. After completion, purge the entire system with nitrogen purge

3. Continue to activate the solid phase extraction column with 20 ml of methanol

4. After completing the third step, pass 10 ml of deionized water to activate the solid phase extraction column.

5. Use a vacuum pump to inject the sample into the SPE column (to ensure the extraction effect, it is recommended to keep the flow rate constant at 10ml/min)

6. Continue to dry the SPE column for 10 minutes using a vacuum pump.

7. The solid phase extraction column was eluted with dichloromethane and cycled 3 times with 10 ml of dichloromethane each time (to ensure optimal results, each elution cycle required a 1 minute interval).

8 Purge the entire piping system with nitrogen to avoid residue.

V. Program setting of Super Vap nitrogen blowing concentration system

1. Preheating temperature: 35 °C

2. Warm-up time: 15min

3. Heating module temperature: 35 ° C

4. Nitrogen blowing pressure: 10 psi

Sixth, experimental test results

Conclusion and analysis

Comparison of the two sets of experimental data shows that the FMS Econotrac simultaneous solid phase extraction system is fully qualified for nitrosamine enrichment extraction in drinking water. Through the combination of simultaneous solid phase extraction and nitrogen blowing concentration system, the seamless connection of extraction and concentration is realized, and the finally obtained sample to be tested is directly concentrated to the gas chromatographic injection bottle without manual transfer to avoid sample loss. At the same time, EconoTrace has a number of functional modules that can quickly expand extraction, purification and concentration to meet different testing requirements.

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