ICP-MS yöntemi ile tırnak örneklerinde Cr, Cu, Zn, As, Se, Sr, Cd, Sb, Hg, Tl, Pb konsantrasyonlarının eş zamanlı belirlenmesi ve zaman içindeki değişkenliği

Yıl 2025, Cilt: 7 Sayı: 3, 257 - 267, 30.09.2025

Esin Akgul Kalkan , Deniz Emre , Selehattin Yılmaz

https://doi.org/10.51435/turkjac.1718104

Öz

Bu çalışmanın amacı, tırnaklardaki 11 metal(oid)i indüktif olarak eşleştirilmiş plazma kütle spektrometrisi (ICP-MS) ile eş zamanlı olarak ölçmek ve ölçümlerin gün içi tekrarlanabilirliğini ve zamana bağlı değişkenliğini göstermektir. Araştırma ekibinde yer alan kadın denekten 2020 yılında iki kez ve 2023 yılında üç kez oje sürülmemiş tırnak örnekleri alındı. Her iki elin tırnakları bir tırnak havuzunda birleştirildi. Her tırnak havuzu bir numune olarak kabul edildi (n= 5). Cr, Cu, Zn, As, Se, Sr, Cd, Sb, Hg, Tl ve Pb'nin eş zamanlı tayini, 3 ardışık gün içi okuma ile gerçekleştirildi. Numunelerin yaşları sırasıyla 1150 ve 939 gün (yaşlı) ve 9, 14 ve 41 gün (güncel numuneler) idi. Üç ardışık günlük ölçümün ortalama bağıl standart sapması (RSD) %5,26, Kendall'ın W değeri ise 0,99 olarak bulundu. Kruskall-Wallis testi üç ölçüm arasında anlamlı bir fark göstermedi (p<.05). Üç yıllık periyotta tekrarlanan ölçümlerde Spearman rho değerleri ve p-değerleri sırasıyla 52Cr (rs=0,884, p=0,000), 63Cu (rs= -0,862, p= 0,000), 66Zn (rs= -0,436, p= 0,104), 75As (rs= -0,840, p= 0,000), 78Se (rs= 0,524, p= 0,045), 88Sr (rs= 0,022, p= 0,938), 111Cd (rs= 0,273, p= 0,325), 121Sb (rs= 0.822, p= 0.000), 201Hg (rs= 0.316, p= 0.251), 205Tl (rs= 0.165, p= 0.557) ve 208Pb (rs= 0.197, p= 0.483) olarak bulundu. Tırnak örneklerinin ICP-MS ile yapılan gün içi ölçümleri yüksek tekrarlanabilirlik ve analitik hassasiyet gösterdi. Element konsantrasyonlarındaki zamana bağlı değişimlerin doğrusal olmadığı ve elementlerin farklı korelasyonlar gösterdiği belirlendi.

Anahtar Kelimeler

Örnek yaşı , Ağır metal , Maruz kalma aralığı , Adli tıp

Simultaneous determination and variability over time of Cr, Cu, Zn, As, Se, Sr, Cd, Sb, Hg, Tl, Pb concentrations in fingernail samples by ICP-MS method

Öz

The aim of this study was to simultaneously quantify 11 metal(oid)s in fingernails by inductively coupled plasma-mass spectrometry (ICP-MS) and to demonstrate the intra-day reproducibility and time-dependent variability of the measurements. Fingernail samples without nail polish were taken from the female subject in the research team twice in 2020 and three times in 2023. The nails of both hands were combined in a nail pool. Each nail pool was considered as one sample (n= 5). Simultaneous determination of Cr, Cu, Zn, As, Se, Sr, Cd, Sb, Hg, Tl, and Pb was carried out with 3 consecutive intra-day readings. The ages of the samples were 1150 and 939 days (aged) and 9, 14, and 41 days (current samples), respectively. The mean relative standard deviation (RSD) of 3 consecutive intraday measurements was 5.26%, and Kendall's W value was 0.99. Kruskall-Wallis test showed no significant difference between the three measurements (p<.05). Spearman rho values and p-values of repeated measurements in 3 years period were found to be 52Cr (rs=0.884, p=0.000), 63Cu (rs= -0.862, p= 0.000), 66Zn (rs= -0.436, p= 0.104), 75As (rs= -0.840, p= 0.000), 78Se (rs= 0.524, p= 0.045), 88Sr (rs= 0.022, p= 0.938), 111Cd (rs= 0.273, p= 0.325); 121Sb (rs= 0.822, p= 0.000), 201Hg (rs= 0.316, p= 0.251), 205Tl (rs= 0.165, p= 0.557) and 208Pb (rs= 0.197, p= 0.483), respectively. Intraday measurements of fingernail samples by ICP-MS showed high reproducibility and analytical precision. It was determined that time-dependent changes in element concentrations were not linear, and the elements showed different correlations.

Anahtar Kelimeler

Age of sample , Heavy metal , Exposure window , Forensic medicine

Etik Beyan

This study was performed in line with the principles of the Declaration of Helsinki. Approval was granted by the Clinical Research Ethics Committee of Çanakkale Onsekiz Mart University (Date: 21 December 2022 / No 2022/16-25).

Teşekkür

This study's ICP-MS analyses were performed at Katip Celebi University Central Research Laboratory (Izmir/Turkey). The authors would like to thank Dr. İslam Cansever for the ICP-MS analyses, and İrem Doğa Akgül for her assistance with the translation.

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