PeerJ analytical chemistry最新文献

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Determination of optical density (OD) of oligodeoxynucleotide from HPLC peak area. HPLC峰面积法测定寡脱氧核苷酸的光密度。
PeerJ analytical chemistry Pub Date : 2022-01-01 Epub Date: 2022-07-07 DOI: 10.7717/peerj-achem.20
Komal Chillar, Yipeng Yin, Adikari M Dhananjani N Eriyagama, Shiyue Fang
{"title":"Determination of optical density (OD) of oligodeoxynucleotide from HPLC peak area.","authors":"Komal Chillar, Yipeng Yin, Adikari M Dhananjani N Eriyagama, Shiyue Fang","doi":"10.7717/peerj-achem.20","DOIUrl":"https://doi.org/10.7717/peerj-achem.20","url":null,"abstract":"Oligodeoxynucleotides (ODNs) are typically purified and analysed with HPLC equipped with a UV-Vis detector. Quantities of ODNs are usually determined using a UV-Vis spectrometer separately after HPLC, and are reported as optical density at 260 nm (OD260). Here, we describe a method for direct determination of OD260 of ODNs using the area of the peaks in HPLC profiles. It is expected that the method will save significant time for researchers in the area of nucleic acid research, and minimize the loss of oligonucleotide samples.","PeriodicalId":93804,"journal":{"name":"PeerJ analytical chemistry","volume":"4 ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9288849/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"40522093","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Extended characterization of petroleum aromatics using off-line LC-GC-MS 离线LC-GC-MS扩展表征石油芳烃
PeerJ analytical chemistry Pub Date : 2021-07-09 DOI: 10.33774/chemrxiv-2021-9rq1k
K. Huynh, Annette E. Jensen, Jonas Sundberg
{"title":"Extended characterization of petroleum aromatics using off-line LC-GC-MS","authors":"K. Huynh, Annette E. Jensen, Jonas Sundberg","doi":"10.33774/chemrxiv-2021-9rq1k","DOIUrl":"https://doi.org/10.33774/chemrxiv-2021-9rq1k","url":null,"abstract":"Characterization of crude oil remains a challenge for analytical chemists. With the development of multi-dimensional chromatography and high-resolution mass spectrometry, an impressive number of compounds can be identified in a single sample. However, the large diversity in structure and abundance makes it difficult to obtain full compound coverage. Sample preparation methods such as solid-phase extraction and SARA-type separations are used to fractionate oil into compound classes. However, the molecular diversity within each fraction is still highly complex. Thus, in the routine analysis, only a small part of the chemical space is typically characterized. Obtaining a more detailed composition of crude oil is important for production, processing and environmental aspects. We have developed a high-resolution fractionation method for isolation and preconcentration of trace aromatics, including oxygenated and nitrogen-containing species. The method is based on semi-preparative liquid chromatography. This yields high selectivity and efficiency with separation based on aromaticity, ring size and connectivity. By the separation of the more abundant aromatics, i.e., monoaromatics and naphthalenes, trace species were isolated and enriched. This enabled the identification of features not detectable by routine methods. We demonstrate the applicability by fractionation and subsequent GC-MS analysis of 14 crude oils sourced from the North Sea. The number of tentatively identified compounds increased by approximately 60 to 150% compared to solid-phase extraction and GC × GC-MS. Furthermore, the method was used to successfully identify an extended set of heteroatom-containing aromatics (e.g., amines, ketones). The method is not intended to replace traditional sample preparation techniques or multi-dimensional chromatography but acts as a complementary tool. An in-depth comparison to routine characterization techniques is presented concerning advantages and disadvantages.","PeriodicalId":93804,"journal":{"name":"PeerJ analytical chemistry","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-07-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47605122","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 3
Impact of heterozygous hemoglobin E on six commercial methods for hemoglobin A1c measurement 杂合血红蛋白E对六种商用血红蛋白A1c测定方法的影响
PeerJ analytical chemistry Pub Date : 2021-03-23 DOI: 10.7717/PEERJ-ACHEM.9
S. Yong, Hong Liu, Cindy Lye Teng Lum, Qian Liu, Sin Ye Sim, Felicia Fu Mun Chay, Wan Ling Cheng, Siew Fong Neo, S. Chew, Lizhen Ong, T. P. Loh, Qinde Liu, T. Teo, S. Sethi
{"title":"Impact of heterozygous hemoglobin E on six commercial methods for hemoglobin A1c measurement","authors":"S. Yong, Hong Liu, Cindy Lye Teng Lum, Qian Liu, Sin Ye Sim, Felicia Fu Mun Chay, Wan Ling Cheng, Siew Fong Neo, S. Chew, Lizhen Ong, T. P. Loh, Qinde Liu, T. Teo, S. Sethi","doi":"10.7717/PEERJ-ACHEM.9","DOIUrl":"https://doi.org/10.7717/PEERJ-ACHEM.9","url":null,"abstract":"\u0000\u0000This study examined the impact of heterozygous HbE on HbA1c measurements by six commonly used commercial methods. The results were compared with those from a modified isotope-dilution mass spectrometry (IDMS) reference laboratory method on a liquid chromatograph coupled with tandem mass spectrometer (LC-MS/MS).\u0000\u0000\u0000\u0000Twenty-three leftover samples of patients with heterozygous HbE (HbA1c range: 5.4–11.6%), and nineteen samples with normal hemoglobin (HbA1c range: 5.0–13.7%) were included. The selected commercial methods included the Tina-quant HbA1c Gen. 3 (Roche Diagnostics, Basel, Switzerland), Cobas B 101 (Roche Diagnostics, Basel, Switzerland), D100 (Bio-Rad Laboratories, Hercules, CA, USA), Variant II Turbo HbA1c 2.0 (Bio-Rad Laboratories, Hercules, CA, USA), DCA Vantage (Siemens Healthcare, Erlangen, Germany) and HbA1c Advanced (Beckman Coulter Inc., Brea, CA, USA).\u0000\u0000\u0000\u0000With the exception of Cobas B 101 and the Variant II Turbo 2.0, the 95% confidence intervals of the Passing–Bablok regression lines between the results from the six commercial methods and the IDMS method overlapped. The latter suggested no statistically significant difference in results and hence no impact on HbA1c result despite the presence of heterozygous HbE. The method of Cobas B 101 gave positive bias at the range of concentrations examined (5.4–11.6%), while that of Variant II Turbo 2.0 gave positive bias at concentrations up to approximately 9.5%. The finding of significant positive bias in the methods of Cobas B 101 and Variant II Turbo 2.0 agrees with the observations of some previous studies, but is contrary to manufacturer’s claim indicating the absence of interference by heterozygous HbE. Our results also clearly showed the impact of heterozygous HbE across a fairly broad measurement range using a laboratory method (the Variant II Turbo 2.0). Laboratory practitioners and clinicians should familiarize themselves with prevailing hemoglobin variants in the population they serve and select the appropriate methods for HbA1c measurement.\u0000","PeriodicalId":93804,"journal":{"name":"PeerJ analytical chemistry","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-03-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46427878","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Screening of 49 antibiotic residues in aquatic products using modified QuEChERS sample preparation and UPLC-QToFMS analysis 改良QuEChERS样品制备及UPLC-QToFMS分析筛选水产品中49种抗生素残留
PeerJ analytical chemistry Pub Date : 2021-02-16 DOI: 10.7717/PEERJ-ACHEM.8
Yao Gao, Tianwen Zhang, Shirong Huang, Xinxin Lin, Sisi Gong, Qiu-fang Chen, Dong-mei Huang, Min Chen
{"title":"Screening of 49 antibiotic residues in aquatic products using modified QuEChERS sample preparation and UPLC-QToFMS analysis","authors":"Yao Gao, Tianwen Zhang, Shirong Huang, Xinxin Lin, Sisi Gong, Qiu-fang Chen, Dong-mei Huang, Min Chen","doi":"10.7717/PEERJ-ACHEM.8","DOIUrl":"https://doi.org/10.7717/PEERJ-ACHEM.8","url":null,"abstract":"A precise analytical method was established for rapid screening of 49 antibiotic residues in aquatic products by ultra-high performance liquid chromatography-quadrupole time of flight mass spectrometry (UPLC-QToFMS). The quick, easy, cheap, effective, rugged and safe (QuEChERS) process was refined for effective sample preparation. The homogenized samples of aquatic products were extracted with 3% acetic acid in acetonitrile, salted out with anhydrous magnesium sulfate and sodium chloride, and cleaned up by octadecylsilane (C18) and primary-secondary amine (PSA) powder. Then, the purified samples were separated on a BEH C18 column using 0.1% formic acid and methanol as mobile phases by gradient elution, detected by MS under positive Electron Spray Ionization (ESI+) mode. The linear range of matrix-matched calibration curve was 1–100 μg/L for each compound with the correlation coefficients in the range of 0.9851–0.9999. The recoveries of target antibiotics at the different spiked levels ranged from 60.2% to 117.9% except for lincomycin hydrochloride, whereas relative standard deviations (RSDs) were between 1.6% and 14.0% except for sulfaguanidine in grass Carp, Penaeus vannamei and Scylla serrata matrices. The limits of detection (LODs) (S/N = 3) for the analytes were 0.05–2.40 μg/kg, 0.08–2.00 μg/kg and 0.10–2.27 μg/kg and the limits of quantification (LOQs) (S/N = 10) were 0.16–8.00 μg/kg, 0.25–6.66 μg/kg and 0.32–7.56 μg/kg in grass Carp, Penaeus vannamei and Scylla serrata, respectively. The method was successfully applied to grass Carp, Penaeus vannamei and Scylla serrata, demonstrating its ability for the determination of multi-categories antibiotic residues in aquatic products.","PeriodicalId":93804,"journal":{"name":"PeerJ analytical chemistry","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-02-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47123461","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 1
Non-target screening of organic compounds in offshore produced water by GC×GC-MS 利用GC×GC-MS对近海采出水中有机化合物进行非靶筛选
PeerJ analytical chemistry Pub Date : 2020-12-07 DOI: 10.26434/chemrxiv.13317938.v1
S. N. Bergfors, K. Huynh, Annette E. Jensen, Jonas Sundberg
{"title":"Non-target screening of organic compounds in offshore produced water by GC×GC-MS","authors":"S. N. Bergfors, K. Huynh, Annette E. Jensen, Jonas Sundberg","doi":"10.26434/chemrxiv.13317938.v1","DOIUrl":"https://doi.org/10.26434/chemrxiv.13317938.v1","url":null,"abstract":"Produced water is the largest by-product of oil and gas production. At off-shore installations, the produced water is typically reinjected or discharged into the sea. The water contains a complex mixture of dispersed and dissolved oil, solids and inorganic ions. A better understanding of its composition is fundamental to (1) improve environmental impact assessment tools and (2) develop more efficient water treatment technologies. The objective of the study was to screen produced water sampled from a producing field in the Danish region of the North Sea to identify any containing organic compounds. The samples were taken at a test separator and represent an unfiltered picture of the composition before cleaning procedures. The analytes were isolated by liquid-liquid extraction and derivatized using a silylation reagent to increase the volatility of oxygenated compounds. The final extracts were analyzed by comprehensive multi-dimensional gas chromatography coupled to a high-resolution mass spectrometer. A non-target processing workflow was implemented to extract features and quantify the confidence of library matches by correlation to retention indices and the presence of molecular ions. Approximately 120 unique compounds were identified across nine samples. Of those, 15 were present in all samples. The main types of compounds are aliphatic and aromatic carboxylic acids with a small fraction of hydrocarbons. The findings have implications for developing improved environmental impact assessment tools and water remediation technologies.","PeriodicalId":93804,"journal":{"name":"PeerJ analytical chemistry","volume":"3 1","pages":"e11"},"PeriodicalIF":0.0,"publicationDate":"2020-12-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46942065","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 3
A simple spectrophotometric evaluation method for the hydrophobic anticancer drug paclitaxel 疏水性抗癌药紫杉醇的简单分光光度评价方法
PeerJ analytical chemistry Pub Date : 2020-03-02 DOI: 10.7717/peerj-achem.3
K. Sugo, M. Ebara
{"title":"A simple spectrophotometric evaluation method for the hydrophobic anticancer drug paclitaxel","authors":"K. Sugo, M. Ebara","doi":"10.7717/peerj-achem.3","DOIUrl":"https://doi.org/10.7717/peerj-achem.3","url":null,"abstract":"In this work, we demonstrate a simple spectrophotometry approach to more accurately quantify and measure paclitaxel (PTX) concentrations. PTX cannot be precisely quantified when mixed with an aqueous solvent, and carries the risk of undergoing crystal precipitation. It is likely that PTX undergoes numerous interactions with aqueous solvents and enters a supersaturated state due to its low solubility. Therefore, a quantitative method is required to measure PTX for quality control before clinical use. Although several high-performance liquid chromatography (HPLC) methods have been reported to date, not all medical facilities have a clinical laboratory with such HPLC devices and analysis techniques. Spectroscopy is a simple and convenient method; however, calibration standards are prepared with an organic solvent, such as methanol and acetonitrile, which, when mixed with PTX, can cause solvent effects that lead to inaccurate results. We generated a calibration curve of PTX at various concentrations (40%, 50%, 60%, 70%, 80%, 90% and 100%) of methanol and evaluated the relative error from HPLC results. The optimum methanol concentration for quantification of PTX was 65.8%, which corresponded to the minimum relative error. The detection limit and quantification limit were 0.030 μg/mL and 0.092 μg/mL, respectively. It was possible to predict the PTX concentration even when polyoxyethylene castor oil and anhydrous ethanol were added, as in the commercially available PTX formulation, by diluting 32-fold with saline after mixing. Our findings show that PTX can be more accurately quantified using a calibration curve when prepared in a methanol/water mixture without the need for special devices or techniques.","PeriodicalId":93804,"journal":{"name":"PeerJ analytical chemistry","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2020-03-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44896021","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 3
Establishing an optimized method for the separation of low and high abundance blood plasma proteins 建立一种分离低丰度和高丰度血浆蛋白的优化方法
PeerJ analytical chemistry Pub Date : 2020-02-10 DOI: 10.7717/peerj-achem.6
Henian Yang, Guijie Wang, Tiantian Zhang, J. Beattie, Shaobo Zhou
{"title":"Establishing an optimized method for the separation of low and high abundance blood plasma proteins","authors":"Henian Yang, Guijie Wang, Tiantian Zhang, J. Beattie, Shaobo Zhou","doi":"10.7717/peerj-achem.6","DOIUrl":"https://doi.org/10.7717/peerj-achem.6","url":null,"abstract":"The study tested the efficiency and reproducibility of a method for optimal separation of low and high abundant proteins in blood plasma. Firstly, three methods for the separation and concentration of eluted (E: low abundance), or bound (B: high abundance) proteins were investigated: TCA protein precipitation, the ReadyPrep™ 2-D cleanup Kit and Vivaspin Turbo 4, 5 kDa ultrafiltration units. Secondly, the efficiency and reproducibility of a Seppro column or a ProteoExtract Albumin/IgG column were assessed by quantification of E and B proteins. Thirdly, the efficiency of two elution buffers, containing either 25% or 10% glycerol for elution of the bound protein, was assessed by measuring the remaining eluted volume and the final protein concentration. Compared to the samples treated with TCA protein precipitation and the ReadyPrep™ 2-D cleanup Kit, the E and B proteins concentrated by the Vivaspin4, 5 kDa ultrafiltration unit were separated well in both 1-D and 2-D gels. The depletion efficiency of abundant protein in the Seppro column was reduced after 15 cycles of sample processing and regeneration and the average ratio of E/(B + E) × 100% was 37 ± 11(%) with a poor sample reproducibility as shown by a high coefficient of variation (CV = 30%). However, when the ProteoExtract Albumin/IgG column was used, the ratio of E/(B + E) × 100% was 43 ± 3.1% (n = 6) and its CV was 7.1%, showing good reproducibility. Furthermore, the elution buffer containing 10% (w/v) glycerol increased the rate of B protein elution from the ProteoExtract Albumin/IgG column, and an appropriate protein concentration (3.5 µg/µl) for a 2-D gel assay could also be obtained when it was concentrated with Vivaspin Turbo 4, 5 kDa ultrafiltration unit. In conclusion, the ProteoExtract Albumin/IgG column shows good reproducibility of preparation of low and high abundance blood plasma proteins when using the elution buffer containing 10% (w/v) glycerol. The optimized method of preparation of low/high abundance plasma proteins was when plasma was eluted through a ProteoExtract Albumin/IgG removal column, the column was further washed with elution buffer containing 10% glycerol. The first and second elution containing the low and high abundance plasma proteins, respectively, were further concentrated using Vivaspin® Turbo 4, 5 kDa ultrafiltration units for 1 or 2-D gel electrophoresis.","PeriodicalId":93804,"journal":{"name":"PeerJ analytical chemistry","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2020-02-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41522073","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 2
Finding a relationship between physicochemical characteristics and ionic composition of River Nworie, Imo State, Nigeria 尼日利亚伊莫州Nworie河的物理化学特征与离子组成之间的关系
PeerJ analytical chemistry Pub Date : 2020-02-04 DOI: 10.7717/peerj-achem.5
E. N. Verla, A. W. Verla, C. Enyoh
{"title":"Finding a relationship between physicochemical characteristics and ionic composition of River Nworie, Imo State, Nigeria","authors":"E. N. Verla, A. W. Verla, C. Enyoh","doi":"10.7717/peerj-achem.5","DOIUrl":"https://doi.org/10.7717/peerj-achem.5","url":null,"abstract":"Water has been described as a universal solvent, and this is perhaps the strength behind its many uses. Despite this unique property, anthropogenic activities along its course and natural factors often determine the composition of water. In the current research, the portion of River Nworie having past Owerri town was sampled in the dry season 2017 to determine its ionic composition at predestinated points and to relate such properties to its physicochemical characteristics. Studies relating physicochemical properties and dissolved toxic ions in water could develop a body of knowledge that could enable detection and quantification of potential risk of ions such as heavy metals from natural water to aquatic ecosystem, animal and human health without actually involving aquatic organism, animal and human. Clean sterile plastic bottles were used for collecting surface water. A total of 30 sub-samples from five points at 300 m apart were sampled in the morning. Physicochemical properties were determined using standard methods and ionic composition of water was determined according methods of APHA. Results revealed that Ca2+ had a mean 23.60 ± 0.67 mg/l and was the highest while K+ with a mean 0.72 ± 0.30 was the least amongst major cations. Amongst the major anions Cl− had mean of 31.58 ± 4.47 mg/l while mean of PO43− was 1.42 ± 0.13 mg/l. The ionic balance calculate as % balance error showed high values for all sampling sites ranging from 30 to 39.42% indicating that there is massive input from anthropogenic activities. The computed relationships for selected heavy metals, cations and anions revealed that R2 values were ranging between  ± 0.012 to 1 indicating some form of relationship existing. The water pH weakly correlated with dissolved cations and anions while moderate with pH only, due to the pH level (5.2–6.2). The cations and anions were more influenced by the water temperature than the heavy metals. Therefore, high temperature ranges of 31–32.4 °C will favour more dissolution of cations and anions in natural water. Cations showed stronger relationship with EC while only heavy metals showed no relationship with DO (Dissolved oxygen). Dissolved oxygen relationship with cations and anions was in the order; K+ > Mg2+ > Ca2+ > Na+ while anions was SO42− > NO3− > Cl− > PO43−, respectively. Information here could be used to predict the effects of using this water for various purposes including water for agricultural purposes, in the management of ion polluted waters, and also to inform on the mitigation process to be taken.","PeriodicalId":93804,"journal":{"name":"PeerJ analytical chemistry","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2020-02-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48744400","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 15
On the mechanism of automated fizzy extraction 自动起泡萃取机理研究
PeerJ analytical chemistry Pub Date : 2019-12-20 DOI: 10.7717/peerj-achem.2
Chun-Ming Chang, Hao-Chun Yang, P. L. Urban
{"title":"On the mechanism of automated fizzy extraction","authors":"Chun-Ming Chang, Hao-Chun Yang, P. L. Urban","doi":"10.7717/peerj-achem.2","DOIUrl":"https://doi.org/10.7717/peerj-achem.2","url":null,"abstract":"Fizzy extraction (FE) facilitates analysis of volatile solutes by promoting their transfer from the liquid to the gas phase. A carrier gas is dissolved in the sample under moderate pressure (Δp ≈ 150 kPa), followed by an abrupt decompression, what leads to effervescence. The released gaseous analytes are directed to an on-line detector due to a small pressure difference. FE is advantageous in chemical analysis because the volatile species are released in a short time interval, allowing for pulsed injection, and leading to high signal-to-noise ratios. To shed light on the mechanism of FE, we have investigated various factors that could potentially contribute to the extraction efficiency, including: instrument-related factors, method-related factors, sample-related factors, and analyte-related factors. In particular, we have evaluated the properties of volatile solutes, which make them amenable to FE. The results suggest that the organic solutes may diffuse to the bubble lumen, especially in the presence of salt. The high signal intensities in FE coupled with mass spectrometry are partly due to the high sample introduction rate (upon decompression) to a mass-sensitive detector. However, the analytes with different properties (molecular weight, polarity) reveal distinct temporal profiles, pointing to the effect of bubble exposure to the sample matrix. A sufficient extraction time (~12 s) is required to extract less volatile solutes. The results presented in this report can help analysts to predict the occurrence of matrix effects when analyzing real samples. They also provide a basis for increasing extraction efficiency to detect low-abundance analytes.","PeriodicalId":93804,"journal":{"name":"PeerJ analytical chemistry","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-12-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43064235","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 6
Analysis of copper, selenium, and zinc in newborn dried bloodspots using total reflection X-ray fluorescence (TXRF) spectroscopy 全反射X射线荧光光谱法分析新生儿干血块中的铜、硒和锌
PeerJ analytical chemistry Pub Date : 2019-11-27 DOI: 10.7717/peerj-achem.1
Jessica Pawly, R. Neitzel, N. Basu
{"title":"Analysis of copper, selenium, and zinc in newborn dried bloodspots using total reflection X-ray fluorescence (TXRF) spectroscopy","authors":"Jessica Pawly, R. Neitzel, N. Basu","doi":"10.7717/peerj-achem.1","DOIUrl":"https://doi.org/10.7717/peerj-achem.1","url":null,"abstract":"There exists great interest in using dried bloodspots across the clinical, public health, and nutritional sciences to characterize circulating levels of essential elements yet current methods face several challenges related to instrumentation, quality control, and matrix effects. Elemental analysis via total X-ray fluorescence (TXRF) may help overcome these challenges. The objective of this study was to develop and apply a novel TXRF-based analytical method to quantify essential elements (copper, selenium, zinc) in dried bloodspots.Analytical methods were developed with human whole blood standard reference materials from the Institut National de Santé Publique du Québec (INSPQ). The method was developed in careful consideration of several quality control parameters (e.g., analytical accuracy, precision, linearity, and assay range) which were iteratively investigated to help refine and realize a robust method. The developed method was then applied to a quantitative descriptive survey of punches (n = 675) taken from residual dried bloodspots from a newborn screening biobank program (Michigan BioTrust for Health).The analytical method developed to quantify the three target elements in dried bloodspots fared well against a priori quality control criteria (i.e., analytical accuracy, precision, linearity and range). In applying this new method, the average (±SD) blood copper, selenium, and zinc levels in the newborn samples were 1,117.0 ± 627.1 µg/L, 193.1 ± 49.1 µg/L, and 4,485 ± 2,275 µg/L respectively. All the elements were normally distributed in the sample population, and the measured concentrations fall within an expected range.This study developed and applied a novel and robust method to simultaneously quantify three essential elements. The method helps overcome challenges in the field concerning elemental analysis in dried bloodspots and the findings help increase understanding of nutritional status in newborns.","PeriodicalId":93804,"journal":{"name":"PeerJ analytical chemistry","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-11-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43046911","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 4
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