Extraction Of Analytes Research Articles

Validation of methods for pesticide residue analysis in milk and milk products asper FSSAI regulation

Accurate analysis of 55 pesticides as per the regulatory requirement of FSSAI for milk and milk products is a challenging task as it requires performing six different types of extractions and detection techniques. Further, before putting to use methods has to be thoroughly validated or checked for its fitness of purpose as per the National or International guidelines to ensure the accuracy of test results. The objective of this study was to develop a validated test method for the determination of55 pesticides in milk and milk products as per FSSAI regulation. QuEChERS based simultaneous extraction of multi class pesticides involves different steps i.e. mixing of reagents, separation of phases, extraction of analytes, clean up followed by reconstitution in suitable solvents. For analysis of few pesticides of different chemical nature, certain analytical steps which are saponification, derivatisation, digestion of analyte to release CS2, extractions using specific solvents, purification usingspecific cartridges at specific pH, temperature and flow conditions are required to be performed. For detection of pesticide residues, mass spectrometry either with gas or liquid chromatography is one of the best approach to meet method performance and validation criteria. In this study, the optimised extraction protocols were investigated for parameters like Linearity, Matrix Effect (ME),Limit of Quantification (LOQ), Specificity, Trueness, Precision, Ion Ratio and Retention Time (RT) to validate the fitness for purpose of the methods. The calibration curves for all the pesticides were linear over the tested range as the concentration of every analyte at each calibration level fall within the residual limit of ±20 %. The LOQ for most of pesticides is established at 5μg/kg, whereas it is 10 μg/kg for Bifenthrin, Cypermethrin,Dichlorvos, Etofenprox, Phorate, Glufosinate Ammonium, and 25μg/kg for Dithiocarbamtes as CS2. The Trueness and Precision of the methods were evaluated by analysing control samples spiked at LOQ and 2 to 10x the RL/LOQ in 6 replicates as per SANTE/11321/2021 guideline. Results for Trueness and Precision meet validation criteria of recovery 70 to 120 % and % RSDr < 20% respectively for all targeted pesticides. The methods fulfilled all other the requirements of SANTE/11321/2021 guidelines and can be extended for routine analysis of pesticide residues in milk and milk products.

Determination of Glyphosate, Its Metabolite, and Glufosinate in Products of Plant Origin by Chromatography–Mass-Spectrometry

A selective procedure is developed for the determination of glyphosate, aminomethylphosphonic acid, and glufosinate in raw materials of plant origin by chromatography–mass spectrometry. The limit of quantification for glyphosate is 0.1 mg/kg and for glufosinate and aminomethylphosphonic acid, 0.4 mg/kg. The procedure is based on the extraction of analytes from a sample with deionized water acidified with hydrochloric acid, solid-phase purification followed by derivatization with 9-fluorenylmethoxycarbonyl chloride, and the additional purification of the derivatives on a sorbent with weak cation-exchange properties. The extraction and purification procedures for the extracts are optimized. The effect of matrix components on the chromatographic separation and detection of glyphosate on chromatographs–mass spectrometers of various types is studied. Validation of the developed procedure showed that the relative expanded uncertainty lies in the range from 15 to 25%.

Overview of Recent Development of Needle-Trap Devices for Analysis of Volatile Compounds

Needle-trap devices (NTDs) are another sorbent-based tool in the haystack of methods used in analytical extractions. Syringe needles, similar to those used for gas chromatography (GC) injection, can be partially filled with suitable sorbents and are used for extracting and collecting volatile organics, followed by injection into a GC instrument via thermal desorption. Although NTDs share many similarities and advantages of solid-phase microextraction (SPME), the larger sorbent bed provides robustness and offers potentially exhaustive extractions. This month, we take a look at the principles and applications of NTDs, and recent developments in their use.

Determination of major and trace elements in plant samples by inductively coupled plasma optical emission spectrometry with deep eutectic solvent extraction based on choline chloride and carboxylic acids.

A rapid, precise, and environmentally friendly approach utilizing an ultrasound assisted deep eutectic solvent-based extraction method was developed for the extraction of Ca, Fe, K, Mg, Mn, Na, P, S and Zn from plant samples. The investigation was conducted on deep eutectic solvents that are based on choline chloride and carboxylic acids. The determination of target analytes in the extracts was carried out using inductively coupled plasma-optical emission spectrometry (ICP-OES). The DESs based on malic acid were found to exhibit the highest extraction recovery values (95-106%). The parameters affecting the extraction of target analytes were optimized using standard reference materials. The target analytes can be effectively extracted from plant samples using 0.5 g of DESs and ultrasonication for 40 minutes. The determination results of the reference samples indicated that the relative error (RE) was below 15.1%, and the relative standard deviation (RSD) was less than 6.3%, demonstrating excellent accuracy and precision. The proposed method was employed to quantify target analytes in actual plant samples. The accuracy of this method was not significantly different from that of the microwave digestion method. The proposed method has been demonstrated to be a valid approach for the determination of target elements in actual plant samples.

Understanding mass hierarchy in different energy loss mechanisms through heavy flavor data

The theoretical analysis of experimental observations, such as the mass hierarchy effect, often neglects some ingredients, which may have a significant impact. The forthcoming measurements at RHIC and LHC will generate heavy flavor data with unprecedented precision, providing an opportunity to utilize high-p⊥ heavy flavor data to analyze the interaction mechanisms in QGP. To this end, we use our recently developed DREENA framework based on the dynamical energy loss formalism. We present: i) How to disentangle the signature of different interaction mechanisms (radiative and collisional energy losses) at the same dataset. ii) Novel observables susceptible to these different mechanisms to be tested by future high-precision measurements. iii) Analytical and numerical extraction of the mass hierarchy effect in energy losses through this observable.

Cancer burden in women with HIV on Medicaid: A nationwide analysis.

Cancer is the leading cause of death in people living with HIV. In the United States, nearly 1 in 4 people living with HIV are women, more than half of whom rely on Medicaid for healthcare coverage. The objective of this study is to evaluate the cancer burden of women living with HIV on Medicaid. We conducted a cross-sectional study of women 18-64 years of age enrolled in Medicaid during 2012, using data from Medicaid Analytic eXtract files. Using International Classification of Diseases, Ninth Revision, Clinical Modification diagnosis codes, we identified women living with HIV (n = 72,508) and women without HIV (n = 17,353,963), flagging the presence of 15 types of cancer and differentiating between AIDS-defining cancers and non-AIDS-defining cancers. We obtained adjusted prevalence ratios and 95% confidence intervals for each cancer and for all cancers combined, using multivariable log-binomial models, and additionally stratifying by age and race/ethnicity. The highest adjusted prevalence ratios were observed for Kaposi's sarcoma (81.79 (95% confidence interval: 57.11-117.22)) and non-Hodgkin's lymphoma (27.69 (21.67-35.39)). The adjusted prevalence ratios for anal and cervical cancer, both of which were human papillomavirus-associated cancers, were 19.31 (17.33-21.51) and 4.20 (3.90-4.52), respectively. Among women living with HIV, the adjusted prevalence ratio for all cancer types combined was about two-fold higher (1.99 (1.86-2.14)) in women 45-64 years of age than in women 18-44 years of age. For non-AIDS-defining cancers but not for AIDS-defining cancers, the adjusted prevalence ratios were higher in older than in younger women. There was no significant difference in the adjusted prevalence ratios for all cancer types combined in the race/ethnicity-stratified analyses of the women living with HIV cohort. However, in cancer type-specific sub-analyses, differences in adjusted prevalence ratios between Hispanic versus non-Hispanic women were observed. For example, the adjusted prevalence ratio for Hispanic women for non-Hodgkin's lymphoma was 2.00 (1.30-3.07) and 0.73 (0.58-0.92), respectively, for breast cancer. Compared to their counterparts without HIV, women living with HIV on Medicaid have excess prevalence of cervical and anal cancers, both of which are human papillomavirus related, as well as Kaposi's sarcoma and lymphoma. Older age is also associated with increased burden of non-AIDS-defining cancers in women living with HIV. Our findings emphasize the need for not only cancer screening among women living with HIV but also for efforts to increase human papillomavirus vaccination among all eligible individuals.

Brief Report: Physician Reimbursement and Retention in HIV Care: Racial Disparities in the US South.

Retention in HIV care remains a national challenge. Addressing structural barriers to care may improve retention. We examined the association between physician reimbursement and retention in HIV care, including racial differences. We integrated person-level administrative claims (Medicaid Analytic eXtract, 2008-2012), state Medicaid-to-Medicare physician fee ratios (Urban Institute, 2008, 2012), and county characteristics for 15 Southern states plus District of Columbia. The fee ratio is a standardized measure of physician reimbursement capturing Medicaid relative to Medicare physician reimbursement across states. Generalized estimating equations assessed the association between the fee ratio and retention (≥2 care markers ≥90 days apart in a calendar year). Stratified analyses assessed racial differences. We varied definitions of retention, subsamples, and definitions of the fee ratio, including the fee ratio at parity. The sample included 55,237 adult Medicaid enrollees with HIV (179,002 enrollee years). Enrollees were retained in HIV care for 76.6% of their enrollment years, with retention lower among non-Hispanic Black (76.1%) versus non-Hispanic White enrollees (81.3%, P < 0.001). A 10-percentage point increase in physician reimbursement was associated with 4% increased odds of retention (adjusted odds ratio 1.04, 95% confidence interval: 1.01 to 1.07). In stratified analyses, the positive, significant association occurred among non-Hispanic Black (1.08, 1.05-1.12) but not non-Hispanic White enrollees (0.87, 0.74-1.02). Findings were robust across sensitivity analyses. When the fee ratio reached parity, predicted retention increased significantly overall and for non-Hispanic Black enrollees. Higher physician reimbursement may improve retention in HIV care, particularly among non-Hispanic Black individuals, and could be a mechanism to promote health equity.

Solidified floating organic drop microextraction procedure based on deep eutectic solvent for the determination of melatonin in pharmaceuticals and dietary supplements

A miniaturized clean-up and preconcentration procedure involving deep eutectic solvent-based solidified floating organic drop microextraction was developed for the determination of melatonin in pharmaceuticals and dietary supplements by high-performance liquid chromatography with UV detection. Melatonin is widely used for the treatment of a large spectrum of diseases, and many studies have focused on its efficacy in reducing COVID-19 severity. For the first time, various hydrophobic deep eutectic solvents based on menthol, medium-chain fatty acids, and long-chain alcohols were studied for the microextraction of melatonin. Among the studied solvents, the deep eutectic solvent based on menthol and heptanoic acid provided the highest extraction recovery (90 %). In the developed procedure, a flat magnetic stirrer bar was covered by a microliter amount of the deep eutectic solvent and the sample solution was added under magnetic stirring. In this case, the deep eutectic solvent phase was easily dispersed into the aqueous phase without the use of any organic disperser solvents, resulting in fast analyte extraction (1 min). In the absence of stirring, the aggregation of extract as a floating drop on the surface of the aqueous phase was observed immediately. The low melting/freezing point and low density of the extraction solvent compared with water allowed one to quickly and easily retrieve a low volume of extract (25 μL) in a microextraction procedure by solidification. Validation of the procedure showed that limits of detection and quantification, calculated from the blank tests based on 3σ and 10 σ, were 0.003 mg g−1 and 0.01 mg g−1, respectively.

Development and validation of LC–MS/MS method for quantification of protease inhibitor Pepstatin A to monitor its robust clearance in vaccine downstream process.

Pepstatin A reversibly inhibits aspartic acid proteases and minimizes the impact of protease-induced degradation in recombinant protein manufacturing process. Pepstatin A is considered as a process-related impurity and must be characterized and controlled during manufacturing. Herein we describe the development and validation of an LC-MS/MS method for the quantitation of pepstatin A to monitor its robust clearance in vaccine purification process. Analyte extraction from process intermediates was carried out using 10% acetonitrile/water extraction method. Acetyl-pepstatin was used as internal standard (IS). Pepstatin A and IS were resolved on a C18 column using 10 mM ammonium acetate in water and methanol/acetonitrile mobile phase system. A triple quadrupole mass spectrometer operating in the positive electrospray ionization mode with multiple reaction monitoring was used to detect Pepstatin A and IS transitions of m/z 686.5 to 229.3 and 644.5 to 229.3, respectively. The method was validated for specificity, linearity, accuracy, repeatability (precision), intermediate precision, and assay robustness. The assay was linear over the range of calibration standards 0.5–100 ng/mL. The Lower-limit-of-quantification (LLOQ) of the method was 0.50 ng/mL.

Association of Family Income With Morbidity and Mortality Among US Lower-Income Children and Adolescents

Family income is known to be associated with children's health; the association may be particularly pronounced among lower-income children in the US, who tend to have more limited access to health resources than their higher-income peers. To investigate the association of family income with claims-based measures of morbidity and mortality among children and adolescents in lower-income families in the US enrolled in Medicaid or the Children's Health Insurance Program. This cross-sectional analysis included 795 000 participants aged 5 to 17 years enrolled in Medicaid (Medicaid Analytic eXtract claims, 2011-2012) living in families with income below 200% of the federal poverty threshold (American Community Survey, 2008-2013). Follow-up ended in December 2021. Family income relative to the federal poverty threshold. Record of International Classification of Diseases, Ninth Revision codes for an infection, mental health disorder, injury, asthma, anemia, or substance use disorder and death record within 10 years of observation (Social Security Administration death records through 2021). Among 795 000 individuals in the sample (all statistics weighted: mean [SD] income-to-poverty ratio, 90% [53%]; mean [SD] age, 10.6 [3.9] years; 56% aged 10 to 17 years), 33% had a diagnosed infection, 13% had a mental health disorder, 6% had an injury, 5% had asthma, 2% had anemia, 1% had a substance use disorder, and 0.6% died between 2011 and 2021, with the mean (SD) age at death of 19.8 (4.2) years. For those aged 5 to 9 years, higher family income was associated with lower adjusted prevalence of all outcomes, except mortality: children in families with an additional 100% income relative to the federal poverty threshold had 2.3 (95% CI, 1.8-2.9) percentage points fewer infections, 1.9 (95% CI, 1.5-2.2) percentage points fewer mental health diagnoses, 0.7 (95% CI, 0.5-0.8) percentage points fewer injuries, 0.3 (95% CI, 0.09-0.5) percentage points less asthma, 0.2 (95% CI, 0.08-0.3) percentage points less anemia, and 0.06 (95% CI, 0.03-0.09) percentage points fewer substance use disorder diagnoses. Except for injury and anemia, the associations were more pronounced among those aged 10 to 17 years than those 5 to 9 years (P for interaction <.05). For those aged 10 to 17 years, an additional 100% income relative to the federal poverty threshold was associated with a lower 10-year mortality rate by 0.18 (95% CI, 0.12-0.25) percentage points. Among children and adolescents in the US aged 5 to 17 years with family income under 200% of the federal poverty threshold who accessed health care through Medicaid or the Children's Health Insurance Program, higher family income was significantly associated with a lower prevalence of diagnosed infections, mental health disorders, injury, asthma, anemia, and substance use disorders and lower 10-year mortality. Further research is needed to understand whether these associations are causal.

Determination of formaldehyde in the daily living environment using membrane-enhanced water plug coupled extraction following peptide-based greener reaction derivatization

Sample preparation methods based on membrane devices represent alternative strategies for analyte extraction from complex samples. Membrane-based microextraction is useful for concentrating and purifying compounds from matrices that are not clean. Formaldehyde pollution has several toxic effects on humans, including genotoxicity, oxidative stress, and carcinogenesis. Herein, an ultrafiltration device equipped with a water plug coupled membrane to trap formaldehyde and quantify free formaldehyde in daily products (such as tableware and craft materials) was used. Formaldehyde was derivatized using a peptide-based green reaction before detection by mass spectrometry. The linear range for formaldehyde detection was 1–100 μg/mL and the detection limit was 0.25 μg/mL. The recovery was 93–104 % and the relative standard deviation and relative error were below 13.9 % for intra-day and inter-day analyses. Formaldehyde was extracted and concentrated in the water plug from sticky samples, such as adhesive, glue, bond, student’s acrylic paint, and cosmetic products. The proposed method was shown to be suitable for free formaldehyde determination in daily-use products. To avoid formaldehyde overexposure, research must focus on materials frequently used in the home environment.

A Gadolinium-Based Magnetic Ionic Liquid for Dispersive Liquid-Liquid Microextraction of Ivermectin from Environmental Water.

The recently introduced gadolinium-based magnetic ionic liquid (Gd-MIL) has been exploited as an extractant in dispersive liquid-liquid microextraction (DLLME) for preconcentration of ivermectin (IVR) from water samples followed by analysis using reversed-phase HPLC with UV detection at 245nm. The utilized Gd-MIL extractant is hydrophobic with markedly high magnetic susceptibility. These features result in an efficient extraction of the lipophilic analyte and facilitate the phase separation under the influence of a strong magnetic field, thus promoting the method sensitivity and increasing the potential for automation. To maximize the IVR enrichment by DLLME, the procedure was optimized for extractant mass, dispersive solvent type/volume, salt addition and diluent pH. At optimized conditions, an enrichment factor approaching 70 was obtained with 4.0-mL sample sizes. The method was validated in terms of accuracy, precision, specificity and limit of quantitation. The method was successfully applied to the determination of IVR in river water samples with a mean relative recovery of 97.3% at a spiked concentration of 400ng/mL. Compared with other reported methods, this approach used a simpler procedure with improved precision, lower amounts of safer solvents and a short analysis time.

Development of two fully automated quick, easy, cheap, effective, rugged, and safe pretreatment methods for the extraction of psychotropic drugs from whole blood samples.

Quick, easy, cheap, effective, rugged, and safe extraction strategies are becoming increasingly adopted in various analytical fields to determine drugs in biological specimens. In the present study, we developed two fully automated quick, easy, cheap, effective, rugged, and safe extraction methods based on acetonitrile salting-out assisted liquid-liquid extraction (method 1) and acetonitrile salting-out assisted liquid-liquid extraction followed by dispersive solid-phase extraction (method 2) using a commercially available automated liquid-liquid extraction system. We applied these methods to the extraction of 14 psychotropic drugs (11 benzodiazepines and carbamazepine, quetiapine, and zolpidem) from whole blood samples. Both methods prior to liquid chromatography-tandem mass spectrometry analysis exhibited high linearity of calibration curves (correlation coefficients,>0.9997), ppt level detection sensitivities, and satisfactory precisions (< 8.6% relative standard deviation), accuracies (within±16% relative error), and matrix effects (81-111%). Method 1 provided higher recovery rates (80-91%) than method 2 (72-86%), whereas method 2 provided higher detection sensitivities (limits of detection, 0.003-0.094ng/mL) than method 1 (0.025-0.47ng/mL) owing to the effectiveness of its dispersive solid-phase extraction cleanup step. These fully automated extraction methods realize reliable, labor-saving, user-friendly, and hygienic extraction of target analytes from whole blood samples.

Novel Validated LC-MS/MS Method For Simultaneous Estimation of Celecoxib and Amlodipine in Rat Plasma and Its Application to A Pharmacokinetic Study

The combination of celecoxib (CLX) and Amlodipine (AMD) was approved for hypertensive patients with osteoarthritis by US-FDA. Hence, a potential analytical method that can simultaneously quantify these two drugs is required. In view of this, a novel and fully validated liquid chromatography-electrospray ionization-tandem mass spectrometric (LC-ESI-MS/MS) method has been established for the quantification of CLX and AMD in rat plasma simultaneously. protein precipitation extraction technique was employed for the extraction of analytes and their deuterated analogues from rat plasma quantitatively. The analytes were separated using the mobile phase comprising of acetonitrile–water with 0.1% formic acid buffer (70:30 v/v) and a flow-rate of 1.0 mL/min and 10 min run time on Agilent SB-C18 analytical column. The multiple reaction monitoring transitions, m/z 504.7→98.1 for CLX, 492.8→129.3 for AMD; 385.6→102.8 for CLX-D4 and 496.8.5→412.3 for AMD-D4 were utilized for the analysis in order to attain high selectivity. The method showed good sensitivity and linearity in the range of the concentration 20–800 ng/mL for CLX and 0.25–10 ng/mL for AMD respectively. Moreover, the method also displayed decent accuracy (87.9-100.27% and 99.28-103.26%) for CLX and AMD and precision according to US-FDA guidelines. The precision values for inter- and intra-day were between 1.92.02-7.085% and 0.083-3.43% and for CLX and AMD respectively. Further, the results of the pharmacokinetic parameters including Cmax, tmax, AUC0-t, AUC0-∞ and t1/2 values of drugs indicated that the developed method is valuable for the successful quantification of the analytes in rat plasma. The developed method is significant and is useful for simultaneous quantification of CLX and AMD.

A new microfluidic-chip device followed by sensitive image analysis of smart phone for simultaneous determination of dyes with different acidic–basic properties

In this study, a new microfluidic-chip coupled with micro solid phase extraction (μ-SPE) and a RGB detection system was designed. The method was used for extraction and simultaneous determination of trace amounts of dyes with different acidic–basic properties. Erythrosine (Ery) and Crystal Violet (CV) were selected as acidic and basic model analytes, respectively. The first step of this method is based on the on-chip electromembrane extraction (CEME) of analytes from aqueous solution. The utilized microfluidic system is a single compartment that composed of three polymethyl metacrylate plates (with sandwiched structures) patterned with palm shaped helix channels. The device consisted one pair of platinum electrodes that were embedded in the acceptor phase channels in each side. The middle part was cut and used as the path of the sample. The extracted analytes by CEME were passed through the micro-packed column containing strong cation and anion exchanger sorbents respectively. Two adsorbents were separated by a polypropylene frit and sealed on each side by two polypropylene frites. Following dye adsorption on the sorbents, the colors that emerged were promptly evaluated using RGB colorimetry on a smartphone. Central composite design was used to analyze and optimize the effective parameters on extraction efficiency. The relative standard deviations (RSDs%) based on five replicate measurements were less than 7.8% for RGB and 8.6% for the spectrophotometry technique under ideal conditions. Image analysis using a smartphone yielded LOD values of 15.0 and 10.5 μg L−1 for Ery and CV, respectively. The CEME- μ-SPE -RGB approach produced findings that were equivalent to those obtained by spectrophotometry. Finally, the approach was used to accurately determine Ery and CV in water samples, yielding good relative recoveries (recovery ≥94.0).

Association of In Utero Antipsychotic Medication Exposure With Risk of Congenital Malformations in Nordic Countries and the US

Psychiatric disorders are common among female individuals of reproductive age. While antipsychotic medication use is increasing, the safety of such medications in pregnancy is an area with large evidence gaps. To evaluate the risk of first-trimester antipsychotic exposure with respect to congenital malformations, focusing on individual drugs and specific malformation subtypes. This cohort study used data from nationwide health registers from the 5 Nordic countries and the US and spanned 1996 to 2018. The Nordic cohort included all pregnancies resulting in singleton live-born infants, and the US cohort consisted of publicly insured mothers linked to their live-born infants nested in the nationwide Medicaid Analytic eXtract. Data were analyzed from November 2020 to April 2022. One or more first-trimester dispensing of any atypical, any typical, and individual antipsychotic drugs. Any major congenital malformation and specific malformation subtypes previously suggested to be associated with antipsychotic exposure in utero: cardiovascular malformations, oral clefts, neural tube defects, hip dysplasia, limb reduction defects, anorectal atresia/stenosis, gastroschisis, hydrocephalus, other specific brain anomalies, and esophageal disorders. Propensity score stratification was used to control for potential confounders. Pooled adjusted estimates were calculated using indirect standardization. A total of 6 455 324 unexposed mothers (mean maternal age range across countries: 24-31 years), 21 751 mothers exposed to atypical antipsychotic drugs (mean age range, 26-31 years), and 6371 mothers exposed to typical antipsychotic drugs (mean age range, 27-32 years) were included in the study cohort. Prevalence of any major malformation was 2.7% (95% CI, 2.7%-2.8%) in unexposed infants, 4.3% (95% CI, 4.1%-4.6%) in infants with atypical antipsychotic drug exposure, and 3.1% (95% CI, 2.7%-3.5%) in infants with typical antipsychotic drug exposure in utero. Among the most prevalent exposure-outcome combinations, adjusted relative risks (aRR) were generally close to the null. One exception was olanzapine exposure and oral cleft (aRR, 2.1 [95% CI, 1.1-4.3]); however, estimates varied across sensitivity analyses. Among moderately prevalent combinations, increased risks were observed for gastroschisis and other specific brain anomalies after atypical antipsychotic exposure (aRR, 1.5 [95% CI, 0.8-2.6] and 1.9 [95% CI, 1.1-3.0]) and for cardiac malformations after chlorprothixene exposure (aRR, 1.6 [95% CI, 1.0-2.7]). While the association direction was consistent across sensitivity analyses, confidence intervals were wide, prohibiting firm conclusions. In this study, considering the evidence from primary and sensitivity analyses and inevitable statistical noise for very rare exposure-outcome combinations, in utero antipsychotic exposure generally was not meaningfully associated with an increased risk of malformations. The observed increased risks of oral clefts associated with olanzapine, gastroschisis, and other specific brain anomalies with atypical antipsychotics and cardiac malformations with chlorprothixene requires confirmation as evidence continues to accumulate.

Carbon Dioxide Microbubble Bursting Ionization Mass Spectrometry.

Aerosols generated by bubble bursting have been proved to promote the extraction of analytes and have ultrahigh electric fields at their water-air interfaces. This study presented a simple and efficient ionization method, carbon dioxide microbubble bursting ionization (CDMBI), without the presence of an exogenous electric field (namely, zero voltage), by simulating the interfacial chemistries of sea spray aerosols. In CDMBI, microbubbles are generated in situ by continuous input of carbon dioxide into an aqueous solution containing low-concentration analytes. The microbubbles extract low- and high-polarity analytes as they pass through the aqueous solution. Upon reaching the water-air interface, these microbubbles burst to produce charged aerosol microdroplets with an average diameter of 260 μm (8.1-10.4 nL in volume), which are immediately transferred to a mass spectrometer for the detection and identification of extracted analytes. The above analytical process occurs every 4.2 s with a stable total ion chromatogram (relative standard deviation: 9.4%) recorded. CDMBI mass spectrometry (CDMBI-MS) can detect surface-active organic compounds in aerosol microdroplets, such as perfluorooctanoic acid, free fatty acids epoxidized by bubble bursting, sterols, and lecithins in soybean and egg, with the limit of detection reaching the level of fg/mL. In addition, coupling CDMBI-MS with an exogenous voltage yields relatively weak gains in ionization efficiency and sensitivity of analysis. The results suggested that CDMBI can simultaneously accomplish both bubbling extraction and microbubble bursting ionization. The mechanism of CDMBI involves bubbling extraction, proton transfer, inlet ionization, and electrospray-like ionization. Overall, CDMBI-MS can work in both positive and negative ion modes without necessarily needing an exogenous high electric field for ionization and quickly detect trace surface-active analytes in aqueous solutions.

Application of electrospun composite nanofibers as an efficient sorbent for extraction of pesticides from food samples

Herein, the composite of polylactic acid (PLA)/ Iron-based metal-organic framework (r-MIL-88A)/ Cellulose electrospun nanofibers was fabricated; and then, applied as a novel sorbent for thin-film micro-extraction (TFME) of four selected pesticides followed by GC-FID analysis. From the evaluation of scanning electron microscopy, Fourier transform infrared spectroscopy energy dispersive X-ray spectroscopy and X-ray diffraction, the successful fabrication of composite nanaofibers was approved. The presence of r-MIL-88A/Cellulose with large surface area and plenty of OH-functional groups results in improving PLA extraction efficiency. The effect of various main parameters on extraction efficiency was evaluated. The LODs (based on S/N = 3) were in the range of 1.0 to 1.5 ng mL−1. Intra-day and inter-day relative standard deviations (RSDs) were in the range of 4.8% - 5.6% and 5.2%-6.4%, respectively. In addition, the fiber to fiber relative standard deviations were observed in the range of 5.2%–12.3%. By using the optimized factors, acceptable linearity ranges were obtained in the range of 3.0-1900.0 ng mL−1 for metribuzin and ethofumasate, and 5.0-2000.0 for atrazine and ametryn (R2 = 0.9913-0.9967). The developed method was investigated in fruit juice, vegetables, milk and honey samples, and recoveries (79.3-95.6%) indicate that the PLA/r-MIL-88A/Cellulose can be a prominent composite film for the extraction of the target analytes in various samples.

Simultaneous Dispersive Liquid–Liquid Microextraction and Determination of Different Polycyclic Aromatic Hydrocarbons in Surface Water

Polycyclic aromatic hydrocarbons (PAHs) are a class of persistent organic pollutants of water, and their determination at trace levels in the aquatic ecosystems is essential. In this work, an ultrasound-assisted dispersive liquid-liquid microextraction (DLLME) procedure was suggested utilizing a binary dispersive agent for recovery of different molecular weight polycyclic aromatic hydrocarbons (PAHs) from waters. The detection was carried out by gas chromatography-mass spectrometry (GC-MS) as well as high-performance liquid chromatography with fluorescence and diode-array detection (HPLC-FD/PDA). The method was optimized for the extraction of analytes with respect to the mixture composition, ratios of components, ultrasonication time and centrifugation parameters. The analytical schemes for PAHs extraction from water samples using different ratios of extraction and dispersive solvents are reported. The mixture consisting of chloroform and methanol was applied for the extraction of PAHs containing two or three fused aromatic rings; the mixture of chloroform and acetonitrile is suitable for PAHs containing more than four aromatic rings. The mixture of chloroform:acetone + acetonitrile was applied in the universal scheme and allowed for the simultaneous extraction of 20 PAHs with different structures. The developed sample preparation schemes were combined with GC-MS and HPLC-FD/PDA, which allowed us to determine the analytes at low concentrations (from 0.0002 µg/L) with the recoveries exceeding 80% and relative standard deviations of about 8%. The developed methods for the determination of 20 PAHs were applied to the analysis of water samples from the Karasun Lake (Krasnodar), Azov Sea (Temryuk) and Black Sea (Sochi).

Neurodevelopmental Problems Not Linked to Antidepressant Exposure In Utero

Neurodevelopmental Problems Not Linked to Antidepressant Exposure In Utero