Name: 다원소 측정을 위한 식품 시료의 균질화 및 산 분해
Uploaded: 2023-12-22T12:50:00
Description: Watch this Scientific Journal Video about Homogenization and Acid Digestion of Food Samples for Multi-Elemental Determination at JoVE.com

homogenization and acid digestion of food samples for multi-elemental determination

다원소 분석을 위한 식품 시료 균질화 및 분해

Elemental analysis is an analytical process for determining the elemental composition of various samples. It can be used to control the intake of metals into human bodies (especially heavy metals1) since their high concentrations may cause unwanted health problems. Heavy metals are also one of the main environmental contaminants, therefore, control of their presence in the environment is necessary2. Moreover, elemental analysis can be employed to determine the geographical origin of food products3 and to control the quality of food and water resources4. In addition, it is used for the determination of micro- and macronutrients in soils5 and to gain insights into geological processes throughout history by examining the chemical composition of minerals and sediments6. Studies have also been made to determine the presence of rare metals in electrical and electronic waste for further metal regeneration7, to evaluate the success of drug treatments8, and to verify the elemental composition of metal implants9.
Inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma optical emission spectroscopy (ICP-OES) are commonly used techniques for the elemental analysis of various samples10. They allow simultaneous determination of multiple elements with limits of detection (LOD) and limits of quantification (LOQ) as low as ng/L. In general, ICP-MS has lower LOD values11 and a wider linear concentration range compared to ICP-OES12. Other techniques to determine elemental composition are microwave-induced plasma optical emission spectrometry13 and several variants of atomic absorption spectroscopy (AAS), including flame atomic absorption spectroscopy, electrothermal atomic absorption spectroscopy2, cold vapor atomic absorption spectroscopy, and hydride generation atomic absorption spectroscopy14. Furthermore, elemental determination with low LOD and LOQ is possible with different electroanalytical methods, especially with anodic stripping voltammetry15,16. Of course, there are other methods to determine the elemental composition of samples, but they are not as frequently employed as the above-mentioned methods.
Direct elemental determination of solid samples is feasible using laser-induced breakdown spectroscopy and X-ray fluorescence17. However, for elemental determination with ICP-MS, ICP-OES, and AAS it is necessary to convert solid samples into a liquid state. For this purpose, acid digestion is performed using acids and auxiliary reagents (in most cases H2O2). Acid digestion is carried out at elevated temperature and pressure, converting the organic part of the sample into gaseous products and converting the metal elements into water-soluble salts, thus dissolving them in the solution18.
There are two main types of acid digestion, open vessel digestion and closed vessel digestion. Open vessel digestion is cost-effective14 but has limitations, such as the maximum digestion temperature, which coincides with the boiling temperature of acids at atmospheric pressure. The sample can be heated on hot plates, heating blocks, water baths, sands baths2, and by microwaves19. By heating the sample in that manner, much of the generated heat is lost to the surroundings20, which extends the digestion time14. Other disadvantages of open vessel digestion include greater chemical consumption, the greater possibility of contamination from the surrounding environment, and possible loss of analytes due to the formation of volatile components and their evaporation from the reaction mixture21.
Closed vessel systems are more convenient for the digestion of organic and inorganic samples compared to open vessel systems. Closed vessel systems utilize a variety of energy sources to heat the samples, such as conduction heating and microwaves22. Digestion methods which use microwaves include microwave-induced combustion23, single reaction chamber systems24, and commonly used microwave-assisted wet acid digestion (MAWD)25,26. MAWD allows digestion at higher operating temperatures, ranging between 220 &#176;C and 260 &#176;C and maximum pressures up to 200 bar, depending on the instrument&#39;s working conditions27.
The efficiency and rate of MAWD depend on several factors, including the chemical composition of the samples, the maximum temperature, the temperature gradient, the pressure in the reaction vessel, the amount of acids added, and the concentration of acids used28. In MAWD, complete acid digestion can be achieved in a few minutes due to the elevated reaction conditions compared to longer-lasting digestions in open vessel systems. Lower volumes and concentrations of acids are required in MAWD, which is in line with current green chemistry guidelines29. In MAWD, a smaller amount of sample compared to open vessel digestion is needed to perform acid digestion, usually up to 500 mg of sample is sufficient30,31,32. Larger sample quantities may be digested, but they require a larger amount of chemicals.
Since the instrument for MAWD automatically controls the reaction conditions and the person does not come in direct contact with the chemicals during heating, MAWD is safer to operate than open vessel digestions. However, the person should always proceed with caution when adding chemicals to the reaction vessels to prevent them from coming into contact with the body and causing harm. Reaction vessels also need to be opened slowly as the pressure is built up inside them during acid digestion.
Although acid digestion is a useful technique for preparing samples for elemental determination, the person performing it should be aware of its possible limitations. Acid digestion may not be suitable for all samples, especially those with complex matrices and those that are highly reactive or could react explosively. Therefore, sample composition should always be evaluated to select the appropriate chemicals and reaction conditions for complete digestion that dissolves all desired elements in the solution. Other concerns that the user must consider, and address are impurities and loss of analytes at every step of sample preparation. Acid digestion must always be performed according to specific rules or using protocols.
The protocol described below provides instructions for the homogenization of food samples in a laboratory-sized mixer, a procedure for cleaning the mixer&#39;s components, properly weighing the sample, adding chemicals, performing acid digestion by MAWD, cleaning the reaction vessels after the digestion is complete, preparing the samples for elemental determination, and performing a quantitative multi-element determination with ICP-MS. By following the instructions given below, one should be able to prepare a sample suitable for elemental determination and perform the measurements of digested samples.

저자 스포트라이트: 식품 샘플의 원소 분석에서 기술 및 과제

ICP-MS를 사용한 다중 원소 측정을 위한 균질화 및 마이크로파 지원 습식 산 분해를 사용한 식품 시료 준비

Our research aims to determine the elemental composition of different food samples using different spectroscopic devices to, for example, control the quality of food samples. Besides ICP-MS, our laboratory can also perform elemental analysis of the digested food samples with ICP-OES, atomic absorption spectroscopy, and ion chromatography. However, we can also perform elemental analysis with X-ray photoelectron spectroscopy, and time-of-flight secondary ion mass spectrometry.Current experimental challenges that we face are mostly in the sample preparation process. Our goal is to improve the sample throughput and to optimize the cleaning procedure to minimize any carryover of the sample. The information in the article is about sample homogenization, acid digestion, and elemental analysis to better understand critical procedures for sample preparation and subsequent analysis as we highlight important steps, suggestions, and limitations of the entire process.We will focus on the optimization of the entire processes for samples such as vegetables, wine, ice creams, E-liquids, and in the future, even inorganic samples, which require different sample preparation techniques.

Watch this Scientific Journal Video about Homogenization and Acid Digestion of Food Samples for Multi-Elemental Determination at JoVE.com

다원소 측정을 위한 식품 시료의 균질화 및 산 분해

시작하려면 깨끗한 세라믹 칼을 사용하여 음식 샘플을 수동으로 더 작은 조각으로 자릅니다. 샘플을 250밀리리터 유리 비커로 옮깁니다. 그런 다음 무게에 변화가 없을 때까지 샘플을 섭씨 105도의 건조기에 넣습니다.다음으로, 건조된 샘플을 믹서 비커로 옮깁니다. 샘플이 미세한 분말 또는 균질한 페이스트로 변할 때까지 갈아줍니다. 깨끗한 플라스틱 주걱을 사용하여 균질화된 샘플을 50밀리리터 유리 비커로 옮깁니다.다음으로, 샘플 250mg을 분석 저울의 열린 반응 용기에 칭량합니다. 칭량이 완료되면 반응 용기를 뚜껑으로 덮습니다. 그런 다음 흄 후드로 옮깁니다.이제 반응 용기의 덮개 뚜껑을 엽니다. 그런 다음 각 반응 용기에 68% 질산 5밀리리터와 30% 과산화수소 1밀리리터를 피펫팅합니다. 200마이크로리터 피펫을 사용하여 스파이크 회수 테스트를 위해 37.5마이크로리터의 ICP 다중 원소 표준 용액을 반응 용기에 추가합니다.스파이크가 없는 샘플과 스파이크가 있는 각 샘플이 세 번에 걸쳐 준비되었는지 확인합니다. 반응 용기에 덮개 덮개를 놓고 반응 용기에 나사산 덮개를 나사로 조여 덮개 덮개를 조입니다. 샘플이 산과 2-3분 동안 반응하도록 합니다.마이크로파 보조 습식 산 분해를 수행하려면 닫힌 반응 용기를 마이크로웨이브 랙에 대칭으로 분배합니다. 랙을 전자레인지 챔버에 삽입하고 홀더에 장착합니다. 그런 다음 전자레인지 도어를 닫습니다.선택한 분해 프로그램을 사용하여 시료를 분해하면서 화면에서 반응 조건의 변화를 모니터링합니다. 소화가 완료되면 오븐 챔버에서 랙을 제거합니다. 악기의 문을 닫고 전원을 끕니다.이제 반응 용기의 뚜껑을 천천히 열어 소화 중에 형성된 가스를 방출합니다. 반응 용기를 흄 후드 쪽으로 돌립니다. 유리 깔때기를 사용하여 분해된 샘플을 깨끗한 25mL 유리 용량 플라스크에 정량적으로 옮깁니다.플라스크의 표시까지 초순수로 샘플을 희석합니다. 그런 다음 마개로 플라스크의 입구를 막고 내용물을 잘 섞습니다. 그런 다음 20밀리리터 플라스틱 주사기를 폴리아미드 주사기 필터에 연결합니다.희석된 샘플로 주사기를 채웁니다. 그런 다음 내용물을 50밀리리터 플라스틱 원심분리기 튜브로 여과합니다. 균질화는 크기가 균일하고 고르게 분포된 미세한 샘플 미립자를 생성했습니다.산성 분해는 시간이 지남에 따라 온도를 꾸준히 상승시켰습니다.

Research

JoVE Journal

Chemistry

Homogenization and Acid Digestion of Food Samples for Multi-Elemental Determination

Preparation of Food Samples Using Homogenization and Microwave-Assisted Wet Acid Digestion for Multi-Element Determination with ICP-MS

Sample preparation is crucial for elemental determination, and various techniques are available, one of which involves homogenization followed by acid ...