Quality evaluation of mycelial Antrodia camphorata using high-performance liquid chromatography (HPLC) coupled with diode array detector and mass spectrometry (DAD-MS)

<p>Abstract</p> <p>Background</p> <p><it>Antrodia camphorata </it>(AC) is an important fungus native to Taiwanese forested regions. Scientific studies have demonstrated that extracts of AC possess a variety of pharmacological functions. This study aims to identify the full profile fingerprint of nucleosides and nucleobases in mycelial AC and to assess the quality of two commercial mycelial AC products.</p> <p>Methods</p> <p>High-performance liquid chromatography coupled with diode array detector and mass spectrometry was employed to identify the major components in mycelial AC. The chemical separation was carried out using a gradient program on a reverse phase Alltima C₁₈AQ analytical column (250 × 4.6 mm, 5 μm) with the mobile phase consisting of deionized water and methanol.</p> <p>Results</p> <p>Ten nucleosides and nucleobases, two maleimide derivatives, and a sterol were identified as the major constituents in mycelial AC. These groups of chemical compounds constitute the first chromatographic fingerprint as an index for quality assessment of this medicinal fungus.</p> <p>Conclusions</p> <p>This study provides the first chromatographic fingerprint to assess the quality of mycelial AC.</p

Medium-term Outcomes of Myocarditis and Pericarditis following BNT162b2 Vaccination among Adolescents in Hong Kong

In this study, we examined the clinical and electrophysiological outcomes of adolescents in Hong Kong who developed myocarditis or pericarditis following BNT162b2 vaccination for COVID-19, and followed-up for 60 to 180 days after their initial diagnosis. Clinical assessments included electrocardiogram (ECG) and echocardiogram at the initial admission and follow-up were compared. Treadmill testing was also performed in some cases. Between 14 June 2021 and 16 February 2022, 53 subjects were approached to participate in this follow-up study, of which 28 patients were followed up for >60 days with a median follow-up period of 100 days (range, 61-178 days) and were included in this study. On admission, 23 patients had ECG abnormalities but no high-grade atrioventricular block. Six patients had echocardiogram abnormalities, including reduced contractility, small rim pericardial effusions, and hyperechoic ventricular walls. All patients achieved complete recovery on follow-up. After discharge, 10 patients (35.7%) reported symptoms, including occasional chest pain, shortness of breath, reduced exercise tolerance, and recurrent vasovagal near-syncope. At follow-up, assessments, including ECGs, were almost all normal. Among the three patients with possible ECG abnormalities, all their echocardiograms or treadmill testings were normal. Sixteen patients (57.1%) underwent treadmill testing at a median of 117 days post-admission, which were also normal. However, at follow-up, there was a significant mean bodyweight increase of 1.81kg (95%CI 0.47-3.1 kg, p=0.01), possibly due to exercise restriction. In conclusion, most adolescents experiencing myocarditis and pericarditis following BNT162b2 vaccination achieved complete recovery. Some patients developed non-specific persistent symptoms, and bodyweight changes shall be monitored

Impact of COVID-19 on cardiovascular testing in the United States versus the rest of the world

Objectives: This study sought to quantify and compare the decline in volumes of cardiovascular procedures between the United States and non-US institutions during the early phase of the coronavirus disease-2019 (COVID-19) pandemic. Background: The COVID-19 pandemic has disrupted the care of many non-COVID-19 illnesses. Reductions in diagnostic cardiovascular testing around the world have led to concerns over the implications of reduced testing for cardiovascular disease (CVD) morbidity and mortality. Methods: Data were submitted to the INCAPS-COVID (International Atomic Energy Agency Non-Invasive Cardiology Protocols Study of COVID-19), a multinational registry comprising 909 institutions in 108 countries (including 155 facilities in 40 U.S. states), assessing the impact of the COVID-19 pandemic on volumes of diagnostic cardiovascular procedures. Data were obtained for April 2020 and compared with volumes of baseline procedures from March 2019. We compared laboratory characteristics, practices, and procedure volumes between U.S. and non-U.S. facilities and between U.S. geographic regions and identified factors associated with volume reduction in the United States. Results: Reductions in the volumes of procedures in the United States were similar to those in non-U.S. facilities (68% vs. 63%, respectively; p = 0.237), although U.S. facilities reported greater reductions in invasive coronary angiography (69% vs. 53%, respectively; p < 0.001). Significantly more U.S. facilities reported increased use of telehealth and patient screening measures than non-U.S. facilities, such as temperature checks, symptom screenings, and COVID-19 testing. Reductions in volumes of procedures differed between U.S. regions, with larger declines observed in the Northeast (76%) and Midwest (74%) than in the South (62%) and West (44%). Prevalence of COVID-19, staff redeployments, outpatient centers, and urban centers were associated with greater reductions in volume in U.S. facilities in a multivariable analysis. Conclusions: We observed marked reductions in U.S. cardiovascular testing in the early phase of the pandemic and significant variability between U.S. regions. The association between reductions of volumes and COVID-19 prevalence in the United States highlighted the need for proactive efforts to maintain access to cardiovascular testing in areas most affected by outbreaks of COVID-19 infection

Determination of oleanolic acid in Caulis clematidis armandii by HPLC

OBJECTIVE: To develop an HPLC method for the content determination of oleanolic acid in Caulis clematidis armandii after hydrolysis. METHODS: In the system of HPLC, a Alltima C_(18)(250 mm×4.6 mm,5 μm) column was used with a mixture of methanol-water-acetic acid-triethylamine(89∶11∶0.04∶0.02) as the mobile phase.The measuring wavelength was set at 207 nm.The flow rate was 1.0 ml·min~(-1) and the column temperature maintained at 45 ℃.RESULTS The oleanolic acid peak in chromatograms was completely separated from ..

Analytical Challenges: Determination of Tetrodotoxin in Human Urine and Plasma by LC-MS/MS

Abstract: Tetrodotoxin (TTX) is a powerful sodium channel blocker found in puffer fish and some marine animals. Cases of TTX poisoning most often result from puffer fish ingestion. Diagnosis is mainly from patient’s signs and symptoms or the detection of TTX in the leftover food. If leftover food is unavailable, the determination of TTX in the patient’s urine and/or plasma is essential to confirm the diagnosis. Although various methods for the determination of TTX have been published, most of them are for food tissue samples. Dealing with human urine and blood samples is much more challenging. Unlike in food, the amount of toxin in the urine and blood of a patient is generally extremely low; therefore a very sensitive method is required to detect it. In this regard, mass spectrometry (MS) methods are the best choice. Since TTX is a very polar compound, there will be lack of retention on conventional reverse-phase columns; use of ion pair reagent or hydrophilic interaction liquid chromatography (HILIC) can help solve this problem. The problem of ion suppression is another challenge in analyzing polar compound in biological samples. This review will discuss different MS methods and their pros and cons. Keywords: TTX poisoning; biological samples; ion suppression; LC-MS/MSMar. Drugs 2011, 9 2292 1

Simultaneous qualitative and quantitative analyses of the major constituents in the rhizome of Ligusticum Chuanxiong using HPLC-DAD-MS.

An HPLC-DAD-MS method was developed for the qualitative and quantitative analysis of the major constituents in Chuanxiong (the dried rhizome of Ligusticum chuanxiong Hort). Twenty compounds including phenolic constituents, alkylphthalides and phthalide dimers were identified using online ESI-MS and comparisons with literature data and standard compounds, and six of them were quantified by HPLC-DAD simultaneously. A comprehensive validation of the method including sensitivity, linearity, repeatability and recovery was conducted. The linear regressions were acquired with R(2) > 0.99 and limit of detection (LOD, S/N = 3) values were between 1.5 and 2.5 ng. The repeatability was evaluated by intra- and inter-day assays, and relative standard deviation (RSD) values were reported within 1.87%. The recovery studies for the quantified compounds were observed in the range of 96.36-102.37% with RSD values less than 2.63%. These phenolic constituents and alkylphthalides, the major constituents in Chuanxiong, are generally regarded as the index for the quality assessment of this herb. The overall procedure is accurate and reproducible, which is considered suitable for the qualitative and quantitative analyses of a large number of Chuanxiong samples

Aristolochic acids detected in some raw Chinese medicinal herbs and manufactured herbal products--a consequence of inappropriate nomenclature and imprecise labelling?

Metadata onlyBACKGROUND: Certain frequently used Chinese herbal medicines commonly used for weight control, may contain toxic Aristolochia species, which have been associated with severe nephropathy and urothelial cancer in humans and animals. The toxic entities in Aristolochia species are aristolochic acid-I (AA-I) and aristolochic acid-II (AA-II). There is a lack of systematic information about the aristolochic acid content of Aristolochia species and related genera, including those in Chinese materia medica that are used in the treatment of overweight individuals. OBJECTIVES: To determine the content of AA-I and AA-II of commonly used Chinese herbal medicines (raw herbs and manufactured products) including species of Aristolochia and related genera. METHODS: Twenty-one raw herbs and seven manufactured herbal products were purchased from herbal wholesalers and traditional Chinese medicinal herb retailers in Melbourne, Australia in September 2003, after the supply of known aristolochic acid-containing herbs and products had been banned in Australia. Six additional raw herbs were sourced from a herbal teaching museum. These were purchased in 2001, before the prohibition. The contents of aristolochic acids of each was determined by high pressure liquid chromatography (HPLC), and confirmed by liquid chromatography-mass spectrometry (LC-MS). RESULTS: Of the samples tested, four of the raw herbs purchased before the ban and two manufactured products purchased after the ban, were found to contain aristolochic acids (16-1002 ppm). CONCLUSIONS: Several Chinese raw herbs and some commercially available manufactured herbal products contain aristolochic acids. The confusion in Chinese nomenclature for related raw herbs, and imprecise labelling of manufactured products may contribute to the inadvertent use of toxic herbal species in Chinese medicine practice. Additional measures are needed to ensure the safety of consumers of Chinese herbal medicines

Assay of free ferulic acid and total ferulic acid for quality assessment of Angelica sinensis.

Activity of Chinese Danggui (DG), the processed root of Angelica sinensis (Oliv.) Diels, is linked to the ferulic acid content but the stability of ferulic acid during extraction for medicinal use is not known. The stabilities of ferulic acid and coniferyl ferulate were evaluated in the extracts of DG using a variety of extraction solvents. These included various combinations and proportions of methanol, water, formic acid, 1 M aqueous hydrochloric acid and 2% sodium hydrogen carbonate (NaHCO3) in water. Coniferyl ferulate was found liable to hydrolyze into ferulic acid in neutral, strongly acidic and basic solvents, where heat and water could facilitate this hydrolysis. However, the hydrolysis was relatively resisted in weakly organic acid. Based on the stability evaluation, two new terms, namely: free ferulic acid and total ferulic acid, were suggested and defined. Free ferulic acid refers to the natural content of ferulic acid in herbs. Total ferulic acid means the sum of free ferulic acid plus the amount of related hydrolyzed components. Meanwhile, the high-performance liquid chromatographic (HPLC) method was developed to assay free ferulic acid and total ferulic acid in DG using methanol-formic acid (95:5) and methanol-2% NaHCO3 in water (95:5) as extraction solvents, respectively. Ten DG samples were investigated on their contents of free and total ferulic acid. The results indicated that the amount variety of free ferulic acid was larger than that of their counterparts, and the ratio of total ferulic acid to free ferulic acid was 4.07 +/- 2.73 (mean +/- SD, n = 10). The chemical assay of DG using total ferulic acid content would be a better choice to assess the herbal quality and was recommended

Determination of free and total available ferulic acid in different types of Chinese angelica by high performance liquid chromatography

Free and conjugated forms of ferulic acid (FA) are generally available in higher plant taxa such as Chinese Angelica (CA, the roots of Angelica sinensis (Oliv.) Diels). These various forms of FA were found readily inter-convertible and the extractable level of each depended on solvent properties and acidity. Extraction efficiency using various pH solutions namely, water, 70% methanol, methanol-formic acid (95:5) and methanol-2% NaHCO3 in water (95:5) was compared. Extractable FA were found varying in samples under neutral solvents extraction, whilst relatively consistent for slightly acidic and alkali solvents which were therefore chosen as the optimal media to extract and determine the reproducible levels of free and total available FA. An accurate and rapid high performance liquid chromatographic (HPLC) analysis was conducted using an Alltima C18 column (5 mum, 4.6 mm i.d. x 250 mm) with a guard column (C18, 5 mum, 4.6 mm i.d. x 7.5 mm) at 30degreesC, eluted with a mixture of 1.0% acetic acid and acetonitrile in a gradient program at a flow rate of 1.0 mL/min and detected at 320 nm. Altogether 20 different types of CA samples including whole root, root head, rootlets, whole root slice, Angelica processed by Chinese yellow wine, and charred Angelica were quantified for free and total available FA. Total available FA was found more abundant than free counterpart with an average ratio of 3.15 (n = 20) in the range of 1.29 to 8.23 for these CA samples. The extraction protocol was proven reliable to quantitatively convert all conjugated FA into its free forms and thereby accurately determined by HPLC method for quality assessment