ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2024
·
IF 3.8
Yan Qiaofang,Huang Fei,Wang Chuyang,Zhan Min,Zhang Qiaoxuan,Huang Di,Yan Jun,Lin Haibiao,Huang Xianzhang,Han Liqiao
Digoxin, a cardiac glycoside, is widely used in the treatment of cardiovascular diseases. Due to its narrow therapeutic range, precise monitoring of its blood concentration is essential. A reference measurement procedure (RMP) is pivotal for ensuring result accuracy and comparability. The RMP for serum digoxin by ID-LC-MS/MS was optimized with sample pre-treatment and detection processes, and the bracketing calibration method was used, which facilitates more accurate measurement, especially for extreme concentrations. The performance of this optimized RMP was thoroughly evaluated. The limit of detection (LoD) was 0.05 ng/mL (0.06 nmol/L) and the lowest limit of quantification (LLoQ) was 0.10 ng/mL (0.13 nmol/L). The intra- and inter-assay imprecisions were 2.24%, 2.51%, 1.40% and 1.72%, 1.65%, 0.97% at 0.5, 2.0, 5.0 ng/mL, respectively. Recoveries were 99.63 to 101.42% and the linear response ranged from 0.1 to 10.0 ng/mL. The relative bias was 0.41% and 2.00% of our results compared with the median of all participating reference laboratories for IFCC-RELA (External Quality Assessment Scheme for Reference Laboratories in Laboratory Medicine) 2023A and 2023B. The uncertainty, calibration and measurement capability (CMC) of this method were also evaluated. The optimized RMP was applied in the Trueness Verification Plan of Southern China, which indicates significant differences among clinical systems, highlighting the need for standardization efforts. In addition, two commonly used clinical systems which employed immunoassay methods were compared with this optimized RMP, and 26 individual serum samples were analyzed. The good correlations indicate the feasibility of standardization for serum digoxin. The optimized RMP serves as an accurate reference baseline for routine methods, aiming to enhance the accuracy and precision of measurements in clinical laboratories. Graphical Abstract
研究领域:
临床化学
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药理学
·
分析化学
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高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2026
·
IF 4.1
Yang Shuang,Wan Wei,Qu Ziyu,Yi Keke,Zhang Di,Jiang You,Ye Zihong,Fang Xiang,Xie Jie,Dai Xinhua
Steroid hormones play crucial regulatory roles in human growth, development, reproduction, and the maintenance of internal environmental homeostasis. Because the concentrations of most hormones in the body are extremely low and their chemical properties vary widely, developing an accurate and sensitive quantitative method has become a primary objective in clinical diagnostics. In this study, an isotope dilution liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS) method was developed and validated for the simultaneous quantification of 22 steroid hormones in human serum. To enhance extraction and purification efficiency, a protein precipitation–solid-phase extraction (PP-SPE) approach was employed, forming a “dual purification” strategy. The limits of quantification for progesterone, cortisol, dihydrotestosterone, and dehydroepiandrosterone sulfate were 0.05, 0.50, 0.05, and 1.00 ng/mL, respectively, representing an improvement over previously reported values obtained using similar sample pretreatment methods. Method validation results demonstrated strong linearity for all 22 steroid hormones ( R 2 > 0.98). Accuracy ranged from 86.9% to 119.5%, intra-day precision was below 9.7%, inter-day precision was below 12.0%, and the matrix effect was controlled within 80.3%–118.1%. These findings indicate that the method is accurate, reliable, and suitable for analyzing multiple components in complex serum matrices. Twenty real serum samples were analyzed to evaluate the clinical applicability of the method. The results demonstrated that this method can be used clinically to monitor steroid hormone levels, assist in diagnosing and treating endocrine disorders, and provide a diagnostic basis for adrenal diseases. It holds significant reference value for clinical laboratory testing. Graphical
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2025
·
IF 3.8
Li Wenya,Gao Bingling,Yang Tao,Tang Liping,Song Dan,Li Hongmei,Sun Keqi,Xiao Peng
3,3′,5-Triiodothyronine (T3) plays a crucial role in the diagnosis and evaluation of thyroid diseases. The current reference measurement procedure (RMP) has been in place for 20 years and is widely adopted by reference laboratories around the world. To enhance the performance of the RMP, we developed and validated a simplified, SI-traceable candidate RMP specifically targeting serum total T3 (TT3) using isotope dilution-liquid chromatography with tandem mass spectrometry (ID-LC–MS/MS). Specifically, T3 reference material was employed as the standard. Compared to the RMP, our method incorporates a simplified serum cleanup process involving protein precipitation and nitrogen drying. The method validation followed ISO guidelines for measurement uncertainty assessment. Our results indicated that there was no significant conversion of T4 into metabolites during the serum pretreatment. The lower limit of the measuring interval was determined to be 0.077 nmol/L, and the regression model was linear across a range of 0.016 to 13.086 nmol/L. The imprecision of intra-assays ranged from 0.1 to 1.9%, while inter-assay imprecision ranged from 0.5 to 1.2%. The bias observed when analyzing SRM971 was between − 0.34 and − 1.65%. This candidate RMP demonstrated excellent agreement with the RMPs developed by RELA activity, showing a mean bias falling within the educational mean ratio (6%). The measurement uncertainties were 0.022 nmol/L for RELA2023A and 0.120 nmol/L for RELA2023B. In conclusion, the developed candidate RMP is traceable, reliable, and easy to operate, showing promising potential for the development of serum reference materials and the standardization of routine assays. Graphical
研究领域:
临床检验学
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内分泌学
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高影响因子
JOURNAL OF MASS SPECTROMETRY
·
2026
·Vol. 61
·期 8
·e70088
·
IF 2.1
Liping Yang,Bingling Gao,Tao Yang,Liping Tang,Ying Kan,Keqi Sun,Peng Xiao
Dehydroepiandrosterone sulfate (DHEAS), a crucial steroid hormone for adrenal function and pubertal development, is highly associated with related diseases. This study aims to develop and validate an isotope dilution liquid chromatography tandem mass spectrometry (ID-LC–MS/MS)-based candidate reference measurement procedure (cRMP) for quantifying serum DHEAS. Serum samples were prepared by protein precipitation with acetonitrile and separated on a reversed phase column. Assay validation was conducted under the guidance of standard documents, including C62-A, EP6-A, EP10-A3, and C50-P endorsed by the Clinical and Laboratory Standards Institute (CLSI). The cRMP was established and proven to be highly specific without significant matrix effect and able to accurately quantify DHEAS in human serum. The intra-assay and inter-assay imprecision ranged from < 0.1 to 1.0% and from 1.0 to 1.1%, respectively. Trueness was assessed by recovery rate from 99.6 to 101.2%. The limit of detection (LoD) was 0.270 nmol/L, and the lower limit of the measuring interval (LLMI) was 12.1 nmol/L. A linear correlation ranged from 7.60 to 41 858 nmol/L was observed with a correlation coefficient > 0.999. R 2 value of linear regression analysis between this method and clinical immunoassays was ≥ 0.990. The relative expanded uncertainty was 1.5%–2.5% over the concentration range of 12.1–33 043 nmol/L. This study developed an ID-LC–MS/MS-based cRMP, which provided high specificity, trueness, and precision for serum DHEAS quantification, contributing to the DHEAS measurement standardization and traceability.
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高影响因子
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