JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2023
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IF 3.4
Lele Wang,Xuezhi Wang,Wenyue Li,Jiajia Liu,Xiukun Yao,Zhiwen Wei,Keming Yun
Phase II metabolites play an important role in diazepam-related cases. The study aimed to assess the stability of diazepam’s phase II metabolites in dried blood spots on filter paper. Methods A piece of filter paper was spotted with 100 µL of whole blood (added 1% sodium fluoride as needed) obtained from participant who received 5 mg diazepam orally, air dried for 2 h at room temperature , and then stored at different conditions. Whole spots were cut at 0.1 cm from the outer edge of blood spots at post-consumption time-points of prior (zero), 5, 16, 35, 61, 120 days and 1, 1.5 years. Analytes were extracted with methanol/water mixture (8:2, v/v) and determined using HPLC-MS/MS. Decomposition rules were analyzed by a statistical software “SPSS”. Results Temazepam glucuronide remained stable (0.5–18.6% loss) at 20 ℃ and at 20 ℃ with 1% sodium fluoride for 16 days, while it was unstable after 5 days at 4 ℃ (21.1–26.2% loss) and − 20 ℃ (28.9 - 34.4% loss). After 35 days, temazepam glucuronide concentrations began to fluctuate significantly under all conditions, and an obvious increase (290.4–355.1%) was observed in 1.5 years. Oxazepam glucuronide was always unstable after 5 days, the percentage loss was even 100% when it was stored for 61 days and 1.5 years. Conclusions Dried blood spots on ordinary filter paper are recommended to be stored at 20 ℃ or 20 ℃ with 1% sodium fluoride within 16 days. Samples should be analyzed immediately or stored in sterile and dry media.
研究领域:
药理学
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法医学
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产品关联
DOI
PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2024
·
IF 3.8
He Ziyun,Dai Haibing,Shen Jian,Huang Yanjie,Liu Jinsong,Yan Renqing,Zhang Feng,Yan Shengkai
17α-Hydroxyprogesterone (17α-OHP) quantification in dried blood spots (DBS) is essential for newborn screening for congenital adrenal hyperplasia (CAH), which is challenging due to its low physiological concentration. The high false-positive rates of immunoassays necessitate the development of more accurate methods. Liquid chromatography tandem mass spectrometry (LC-MS/MS) offers increased specificity and sensitivity, yet standardized procedures for 17α-OHP measurement are required for clinical application. A candidate reference measurement procedure (cRMP) using isotope dilution LC-MS/MS was developed for 17α-OHP quantification in DBS. By utilizing stable isotope-labeled D8-17α-OHP as an internal standard, the cRMP was optimized, covering sample preparation, calibration, and LC-MS/MS analysis. The method performance was validated across several parameters, including precision, accuracy, specificity, detection limits, and matrix effects. Clinical applicability was further assessed through the establishment of reference intervals for healthy newborns. The developed cRMP exhibited a linear range of 1.00 to 80.00 ng/mL for 17α-OHP, with detection and quantification limits of 0.14 ng/mL and 0.52 ng/mL, respectively. Inter- and intraday precision demonstrated coefficients of variation within 1.27 to 5.69%. The recovery rates and matrix effects were well within acceptable limits, ensuring method reliability. Clinical application showed distinct reference intervals for healthy newborns that were unaffected by sex but influenced by weight and gestational age. This method significantly enhances CAH diagnostic accuracy in newborns, providing a valuable tool for clinical laboratories and improving newborn screening program standardization and traceability.
研究领域:
医学检验
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临床化学
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产品关联
DOI
PubMed
高影响因子
Forensic Toxicology
·
2023
·Vol. 41
·期 2
·241-248
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IF 2.2
Guo Caixia,Yan Hui,Liu Wei,Xiang Ping,Di Bin,Shen Min
Purpose An analytical method using liquid chromatography with tandem mass spectrometry (LC–MS/MS) was established and validated for screening 425 drugs and poisons in dried blood spots (DBSs). Methods Blood (20 μL) was spotted on Whatman FTA™ classic card to prepare DBS sample, then extracted with 150 μL methanol and analyzed by LC–MS/MS using a multiple reaction monitoring method. Results The limit of detection of the compounds were 0.1–10 ng/mL. The values for recovery and matrix effect were 40.3–114.9% and 40.2–118.4%, respectively. This method was successfully applied to DBS samples from 105 humans suspected of drug poisoning, which was stored for 3–5 years at room temperature. Thirty-three kinds of drugs, including benzodiazepines, antipsychotics, antidepressants, antipyretic analgesics, non-steroidal anti-inflammatory drugs, antibiotics, antiepileptic drugs, new psychoactive drugs were confirmed in 102 cases, while no compound was detected in the other 3 cases. Estazolam, a benzodiazepine widely used in clinical practice as a sedative, hypnotic, and anti-anxiety drug, was the most frequently detected substance, occurring in 34.2% of the cases. Conclusions Most drugs in DBS could still be detected after storage for 3–5 years, but ambroxol, zopiclone, carbofuran, chlorpyrifos, and valproic acid were not detectable after 3–5 years of storage at room temperature. The components measured in DBS were consistent with those measured in whole blood at the collection time, thereby confirming that DBS samples have the advantage of stable storage at room temperature.
研究领域:
分析化学
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法医学
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药理学
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DOI
PubMed
高影响因子
CLINICAL BIOCHEMISTRY
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2025
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IF 2.1
Chunyan Zhang,Nan Bai,Yanling Yang,Yuxuan Cheng,Xiyu He,Meng Wang,Honghui Zhou,Yaping Tian
Objectives Metabolic disorders in newborns can cause significant morbidity and mortality if not diagnosed and managed early. In this study, we developed and validated a reliable LC-MS/MS method to simultaneously quantify methylmalonic acid, methylcitric acid, malonic acid, ethylmalonic acid, and total homocysteine associated with metabolic disorders. Design and methods According to Clinical Laboratory Standards Institute (CLSI) guidelines, various analytical performances (i.e., precision, linearity, accuracy and reference intervals) were rigorously evaluated. Meanwhile, sample preparation, chromatographic separation and mass spectrometric detection and incorporating stable isotope-labeled internal standards were optimized. Furthermore, calibrators and quality controls were developed to ensure standardization and traceability. Results The coefficient of variations for precision were less than 10.0 %. Meanwhile, the results showed high accuracy (recoveries: 94.57 %–109.60 %) and robust linearity (R 2 > 0.9935) over clinically relevant ranges. The limits of detection and limits of quantification for all analytes were established, enabling sensitive detection of pathological elevations. Reference intervals for pediatric populations (ages 0–1 month and 2 months to 18 years) were determined, providing essential baselines for clinical interpretation. Conclusions The newly developed method demonstrated good analytical performance and offers a standardized, high-throughput solution for clinical laboratories to improve early diagnosis and personalized management of metabolic diseases.
研究领域:
临床化学
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代谢组学
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新生儿筛查
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质谱分析
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生物医学检验
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产品关联
DOI
PubMed
高影响因子
Advanced Science
·
2024
·Vol. 11
·期 15
·2305701
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IF 14.3
Haiyang Su,Huiwen Zhang,Jiao Wu,Lin Huang,Mengji Zhang,Wei Xu,Jing Cao,Wanshan Liu,Ning Liu,Hongwei Jiang,Xuefan Gu,Kun Qian
Phenylketonuria (PKU) is the most common inherited metabolic disease in humans. Clinical screening of newborn heel blood samples for PKU is costly and time-consuming because it requires multiple procedures, like isotope labeling and derivatization, and PKU subtype identification requires an additional urine sample. Delayed diagnosis of PKU, or subtype identification can result in mental disability. Here, plasmonic silver nanoshells are used for laser desorption/ionization mass spectrometry (MS) detection of PKU with label-free assay by recognizing metabolic profile in dried blood spot (DBS) samples. A total of 1100 subjects are recruited and each DBS sample can be processed in seconds. This platform achieves PKU screening with a sensitivity of 0.985 and specificity of 0.995, which is comparable to existing clinical liquid chromatography MS (LC-MS) methods. This method can process 360 samples per hour, compared with the LC-MS method which processes only 30 samples per hour. Moreover, this assay enables precise identification of PKU subtypes without the need for a urine sample. It is demonstrated that this platform enables high-performance and fast, low-cost PKU screening and subtype identification. This approach might be suitable for the detection of other clinically relevant biomarkers in blood or other clinical samples.
研究领域:
医学诊断
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质谱分析
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代谢组学
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临床化学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF THE AMERICAN SOCIETY FOR MASS SPECTROMETRY
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2025
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IF 2.7
Shuo Cao,Xinrong Jiang,Xiaoming Chen,Xuetong Qu,Jianmin Wu
Acylcarnitines (ACs), essential intermediates in fatty acid β-oxidation, are increasingly recognized as biomarkers for inborn errors of metabolism (IEM), insulin resistance, heart failure, and neurodegenerative diseases. However, conventional liquid chromatography–mass spectrometry (LC-MS) and flow injection–mass spectrometry (FI-MS) methods are hindered by complex sample preparation, limited throughput, and matrix interferences. Meanwhile, matrix-assisted laser desorption/ionization–MS (MALDI-MS) suffers from low-mass background noise and poor reproducibility. Here, we present a dual-innovation mass spectrometry platform combining a substrate composed of sulfonic acid–gold nanoparticle-decorated silicon nanowires (Sulfo-Au-SiNWs) for electrostatic adsorption-laser desorption/ionization (EALDI) and a full-spectrum internal standard (FS IS) strategy based on d6-ethanol derivatization. The optimized Sulfo-Au-SiNWs offer uniform crystallinity, in situ electrostatic enrichment, efficient thermal desorption, and gold-mediated charge–hole separation, resulting in a ∼300% increase in AC signal intensity. This enabled the selective detection of over ten medium- and long-chain ACs that were previously undetectable using unmodified SiNWs. The FS IS method incorporates over 30 derivatized AC species, enabling simultaneous quantification with detection limits below 0.01 μmol/L, surpassing the sensitivity of traditional FI-MS. The platform delivers spike recovery rates of 96–112% and supports high-throughput analysis, processing each sample within seconds. Validation against FI-ESI-MS/MS in both urine and dried blood spot samples demonstrated excellent agreement (ρ > 0.95) and effectively identified IEM patient profiles via statistically significant AC elevations. With strong intra- and interbatch precision (median RSD < 12.5%) and substrate stability exceeding one month, this EALDI-MS/FS IS workflow provides a high-throughput, high-coverage, and quantitatively robust solution for clinical AC profiling and newborn screening.
研究领域:
质谱分析
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临床诊断
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代谢组学
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生物标志物发现
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新生儿筛查
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分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2023
·
IF 3.4
Jianmei Lv,Qiping Wu,Sanwang Li,Hanxi Yi,Feifan Xie
Bacterial infection is a leading cause of neonatal death . Ceftazidime , commonly used for neonatal infections , is often used off-label. Blood sampling limits pharmacokinetic (PK) studies in neonatal patients. The dried blood spots (DBS) are a potential matrix for microsampling. Herein, we describe an ultra-performance liquid chromatography with a photodiode array (UPLC-PDA) to determine ceftazidime in DBS from neonatal patients in support of pharmacokinetic studies. The Capitainer® device-based DBS samples containing 10 µL blood were extracted in 70% methanol/water ( v/v ) with acetaminophen as the internal standard (IS). The extraction process was carried out at 20 °C using a block bath shaker at 1000 rpm for 30 min. The extracted ceftazidime was subsequently eluted through an Acquity UPLC HSS T3 column (2.1 × 50 mm, 1.8 µm). Elution was achieved using a water (containing 0.1% trifluoroacetic acid)/acetonitrile linear gradient at a flow rate of 0.5 mL/min, and the analytical time was 3.2 min. The PDA detection wavelength was set at 259 nm. The method underwent thorough validation following the recommendation of the European Bioanalysis Forum (EBF) and the bioanalytical guideline established by the European Medicines Agency (EMA). No interfering peaks were detected at the retention times of ceftazidime and IS. The ceftazidime exhibited a quantification range spanning from 0.5 to 200 µg/mL, and the assay demonstrated good accuracy (intra/inter-assay ranging from 90.1% to 104.8%) and precision (intra/inter-assay coefficient of variations ranging from 4.8% to 11.7%). The method's applicability was demonstrated by analyzing clinical DBS samples collected from neonatal patients.
研究领域:
药理学
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分析化学
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新生儿学
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临床研究
✓ 已验证
产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）