Inter-day Tests Research Articles

Carbonized silk fibers for in-tube solid-phase microextraction to detect polycyclic aromatic hydrocarbons in water samples.

Silk fibers were carbonized to develop a biomass carbon material as an adsorbent for solid-phase microextraction. The surface structure of the carbonized silk fibers was characterized by scanning electron microscopy, and the graphitization degree was determined by Raman spectrometry. After carbonization under high temperature, the orderliness and structural regularity of carbon atoms on silk fibers were promoted. Extraction tube packed with carbonized silk fibers was prepared for in-tube solid-phase microextraction. Coupled with high performance liquid chromatography, it exhibited good extraction performance for hydrophobic polycyclic aromatic hydrocarbons. Main parameters including sampling volume, sampling rate, methanol content in sample, and desorption time were systematically investigated. Under the optimum conditions, the analysis method was established and it exhibited wide linear range (0.016-20 μg/L) with good linearity (correlation coefficient ≥ 0.9947), low limits of detection (0.005-0.050 μg/L), and high enrichment factors (1189-2775). Relative standard deviations (n=3) for intraday (≤3.3%) and interday (≤9.6%) tests indicated that the extraction material had satisfactory repeatability. Finally, the analytical method was successfully applied to detect trace polycyclic aromatic hydrocarbons in real water samples, demonstrating its satisfactory practicability.

Ultrasound assisted combined molecularly imprinted polymer for the selective micro-solid phase extraction and determination of aflatoxins in fish feed using liquid chromatography-tandem mass spectrometry

A combined procedure based on using ultrasounds for target isolation followed by porous membrane-protected micro solid phase extraction using a molecularly imprinted polymer as an adsorbent has been developed as a highly selective extraction and clean-up procedure for isolating aflatoxins B1, B2, G1, and G2 from fish feed before ultra-high-performance liquid chromatography tandem mass spectrometry determination. Polymeric adsorbent beads have been synthesized by the precipitation polymerization method which guarantees a homogeneous particles size distribution and the integrity of the generated imprinted cavities. In addition, polymerization was performed using a higher proportion of organic solvent (toluene) in the porogen mixture, which generates MIP particles adequate for interacting with targets dissolved in organic (hydro-organic) mixtures (extracts from fish feed). These approaches led to a selective and high efficient pre-concentration method for AFs. Ultrasound-assisted extraction (10 mL of 60:40 acetonitrile/0.1 M KH2PO4 pH 6.0, 40% amplitude, continuous sonication for 7.0 min) allowed an efficient aflatoxins isolation from fish feed. In addition, the resulting pH of the extract (pH 7.0) has been found to be the optimum for performing clean-up/pre-concentration (enrichment factor of 33.3) by molecularly imprinted polymer based micro-solid phase extraction (orbital horizontal shaking speed at 150 rpm for 10 min for loading, and 5 mL of 95:5 acetonitrile/formic acid as eluting solution using ultrasounds 35 kHz for 15 min). The current proposal was shown to be an accurate and precise method through relative standard deviation of intraday and inter-day tests below 20% and analytical recoveries in the range of 80–100%. The limits of detection were within the 0.42–1.15 μg kg−1 range, quite lower than those established by European Commission guidelines for aflatoxins in animal feeds.

Curcumin nanoparticle doped starch thin film as a green colorimetric sensor for detection of boron

A tapioca starch film doped with curcumin nanoparticles was successfully fabricated and applied as a novel green colorimetric sensor for detection of boron in wastewater. Curcumin nanoparticles (curn, 30-90 nm) extracted from turmeric powder were used as a green probe, while tapioca starch was used as a natural support substrate. A yellow thin film (51 μm thick) fabricated on a used plastic spoon turned red-brown after immersion in boron solution (pH 9) for 15 min with excellent selectivity. The film costs only 0.0007 USD, while the cost of the sensor (curn-film on new plastic spoon) was 0.004 USD. After use the film could be completely washed from the plastic, it being biodegradable, while the used plastic spoon could be re-used to fabricate a new sensor at least 10 times. The good 1.52%RSD precision was obtained across three lots fabricated. When the curn-film was used in conjunction with digital image colorimetry (DIC), a simple and rapid quantification of boron was achieved. The green color layer in reflected light image of the red-brown product (IG) provided the highest sensitivity (64 ± 1 a.u. L mg-1) and the lowest detection limit of 0.052 ± 0.001 mg L-1. The intra-day testing (9 films) had 2.41 to 4.34%RSD, while the inter-day testing had 2.29 to 5.66%RSD (15 films, 5 days). Accuracy in terms of relative error for control samples (0.40 mg L-1) was+3.63%. Wastewater samples from Para-rubber wood processing plant were quantified by curn-film and DIC, giving 4248 ± 391 mg L-1 boron concentration with no significant difference to ICP determination at 95% confidence level. The sensors after storage in a desiccator for a year gave readings changed by only+3.5% and-2.1% relative to freshly prepared sensors.

Baseline separation of α and β-acids homologues and isomers in hop (Humulus lupulus L.) by CD-MEKC-UV.

An alternative method for simultaneous baseline separation of α and β-acids homologues and isomers in hop by CD-MEKC with UV detection was proposed. The optimized background electrolyte was composed of 30mmol/L sodium tetraborate solution, 45mmol/L sodium dodecyl sulfate, 20mmol/L β-cyclodextrin and 10% v/v acetonitrile. The instrumental conditions were evaluated by using a 33 Box-Benhken experimental design. In order to demonstrate the applicability of the method, 21 hop samples from different varieties were analyzed. The repeatability intra- and interday tests were performed and relative standard deviations lower than 7% for area and migration times were observed. The present method comprehended 8min analysis time and revealed to be faster and more efficient when compared to previous reports from literature.

Bare polyprolylene hollow fiber as extractive phase for in-tube solid-phase microextraction to determine estrogens in water samples.

Polypropylene hollow fibers as the adsorbent were directly filled into a polyetheretherketone tube for in-tube solid-phase microextraction. The surface properties of hollow fibers were characterized by a scanning electron microscope. Combined with high performance liquid chromatography, the extraction tube showed good extraction performance for five environmental estrogen hormones. To achieve high analytical sensitivity, four important factors containing sampling volume, sampling rate, content of organic solvent in sample, and desorption time were investigated. Under the optimum conditions, an online analysis method was established with wide linear range (0.03-20µg/L), good correlation coefficients (≥0.9998), low limits of detection (0.01-0.05µg/L), low limits of quantitation (0.03-0.16µg/L), and high enrichment factors (1087-2738). Relative standard deviations (n=3) for intraday (≤3.6%) and interday (≤5.1%) tests proved the stable extraction performance of the material. Durability and chemical stability of the extraction tube were also investigated, relative standard deviations of all analytes were less than 5.8% (n=3), demonstrating the satisfactory stability. Finally, the method was successfully applied to detect estrogens in real samples.

Application of UPLC-MS/MS to simultaneously detect four bioactive compounds in the tumour-shrinking decoction (FM1523) for uterine fibroids treatment.

The Chinese medicine formulation, tumour-shrinking decoction (TSD, FM1523), which consists of 15 natural medicines, is used for uterine fibroids (UFs) therapy and possesses excellent clinical therapeutic effect. To develop a sensitive and validated analytical method for the simultaneous quantification of four crucial bioactive compounds including isorhamnetin-3-O-neohesperidoside, curcumin, peimine and tetrahydropalmatine in the principal formulation of this decoction. An ultra-performance liquid chromatography coupled tandem mass spectrometry (UPLC-MS/MS) with an electrospray ionisation (ESI) source in multiple reaction monitoring (MRM) mode was conducted to investigate these bioactive compounds in the TSD. The chromatographic separation was performed on a C18 column when the flow rate was adjusted at 0.2mL/min with gradient elution of acetonitrile-water with 0.1% formic acid. Accelerated solvent extraction (ASE) method with higher extraction efficiency was employed for TSD sample pre-treatment. The linearity, limit of detection (LOD) and limit of quantification (LOQ) were determined for this analytical method. The mean recoveries of the compounds were determined between 100.23% and 104.02% with satisfactory relative standard deviation (RSD) in the ranges of 2.65% to 3.81%. The precision was evaluated by intra-day and inter-day tests, which revealed RSD within the ranges of 1.21% to 2.14% and 1.24% to 2.32%, respectively. The bioactive compounds of TSD samples were successfully quantified via UPLC-MS/MS with MRM mode. This study could help to evaluate the pharmacokinetic study of TSD during clinical applications and present a facile strategy for quantifying bioactive compounds in traditional Chinese Medicine decoction.

Inter-day test–retest reliability and feasibility of isokinetic, isometric, and isotonic measurements to assess quadriceps endurance in people with chronic obstructive pulmonary disease: A multicenter study

The aims were to determine reliability and feasibility of measurements to assess quadriceps endurance in people with chronic obstructive pulmonary disease. Sixty participants (forced expiratory volume in one second (mean ± standard deviation) 55 ± 18% of predicted, age 67 ± 8 years) were tested in an inter-day, test–retest design. Isokinetic, isometric, and isotonic protocols were performed using a computerized dynamometer. Test–retest relative and absolute reliability was determined via intraclass correlation coefficient (ICC), coefficient of variation (CV%), and limits of agreement (LoA%). Isokinetic total work demonstrated very high relative reliability (ICC: [95% confidence interval] = 0.98 [0.94–0.99]) and the best absolute reliability (CV% (LoA%) = 6.5% (18.0%)). Isokinetic fatigue index, isometric, and isotonic measures demonstrated low-to-high relative reliability (ICC = 0.64 [0.46–0.77], 0.88 [0.76–0.94], 0.91 [0.85–0.94]), and measures of absolute reliability (CV% (LoA%)) were 20.3% (56.4%), 14.9% (40.8%), and 15.8% (43.1%). For isokinetic total work and isometric measurements, participants performed better on retest (4.8% and 10.0%, respectively). The feasibility was similar across protocols with an average time consumption of less than 7.5 minutes. In conclusion, isokinetic, isometric, and isotonic measurements of quadriceps endurance were feasible to a similar extent and presented low-to-very high relative reliability. Absolute reliability seems to favor isokinetic total work measurements.

Simultaneous determination of sodium iron chlorophyllin and sodium copper chlorophyllin in food using high-performance liquid chromatography and ultra-performance liquid chromatography-mass spectrometry.

A simultaneous method for analyzing sodium iron chlorophyllin (SIC) and sodium copper chlorophyllin (SCC) using high-performance liquid chromatography was developed. This method employed an Inertsil ODS-2 column and diode array detection at 395 nm, using methanol-water (97:3 and 80:20, v/v) containing 1% acetic acid as the mobile phase. Liquid chromatography-tandem mass spectrometry was used to identify the main components of SIC and SCC as Fe-isochlorine e4 and Cu-isochlorine e4, respectively. The limits of detection and quantitation of SIC were 1.2 and 4.1 mg/kg, respectively, while those of SCC were 1.4 and 4.8 mg/kg, respectively. For intraday and interday tests, the SIC recoveries from candy ranged from 81% to 101%, while SCC recoveries ranged from 100% to 109%. The developed method can be applied to the rapid determination of SIC and SCC in candy.

Magnetic framework composite as sorbent for magnetic solid phase extraction coupled with high performance liquid chromatography for simultaneous extraction and determination of tricyclic antidepressants

In this study, magnetic framework composites (MFCs) (Fe3O4@TMU-10) microspheres were successfully fabricated and applied as an effective sorbent for preconcentration of the two model tricyclic antidepressants (TCAs) amitriptyline and imipramine from biological samples. MFCs were fabricated by a step-by-step assembly, novel, simple and efficient strategy. The shell thickness of the Metal-organic frameworks (MOFs) could also be easily controlled by tuning the number of assembly cycles. By coupling magnetic solid-phase extraction (MSPE) with high-performance liquid chromatography with UV detector (HPLC-UV), a simple, reliable, fast, sensitive and cost-effective method for simultaneous determination of TCAs was developed. Under optimal conditions, the preconcentration factors and relative recoveries of the studied compounds were obtained in the range of 43–50 and 90.5–99.0% respectively. The calibration curves were obtained in the range of 5–800 μg L−1 with reasonable linearity (R2 > 0.9904) and the limits of detection (LODs) ranged between 2 and 4 μg L−1 (based on S/N = 3). The relative standard deviations of intra- and inter-day tests ranged from 3.1 to 4.6% and from 4.3 to 5.2%, respectively. The results demonstrate that Fe3O4@TMU-10 core–shell magnetic microspheres combine advantages of MOFs and magnetic nanoparticles, and are the promising sorbents for rapid and efficient extraction of target analytes from urine and plasma complex biological samples.

Intra-session and Inter-day Reliability of the Myon 320 Electromyography System During Sub-maximal Contractions.

Electromyography systems are widely used within the field of scientific and clinical practices. The reliability of these systems are paramount when conducting research. The reliability of Myon 320 Surface Electromyography System is yet to be determined. This study aims to determine the intra-session and inter-day reliability of the Myon 320 Surface Electromyography System. Muscle activity from fifteen participants was measured at the anterior deltoid muscle during a bilateral front raise exercise, the vastus lateralis muscle during a squat exercise and the extensor carpi radialis brevis (ECRB) muscle during an isometric handgrip task. Intra-session and inter-day reliability was calculated by intraclass correlation coefficient, standard error of measurement and coefficient of variation (CV). The normalized root mean squared (RMS) surface electromyographic signals produced good intra-session and inter-day testing intraclass correlation coefficient values (range: 0.63–0.97) together with low standard error of measurement (range: 1.49–2.32) and CV (range: 95% Confidence Interval = 0.36–12.71) measures for the dynamic-and-isometric contractions. The findings indicate that the Myon 320 Surface Electromyography System produces good to fair reliability when examining intra-session and inter-day reliability. Findings of the study provide evidence of the reliability of electromyography between trials which is essential during clinical testing.

A Light-Up Probe for Detection of Adenosine in Urine Samples by a Combination of an AIE Molecule and an Aptamer.

A light-up fluorescent probe for the detection of adenosine was constructed with an AIE (aggregation-induced emission) molecule and a DNA aptamer. The AIE molecule was used as a signal generator, and the DNA aptamer was used as a recognition element for adenosine. The emission of the AIE molecule was due to its intramolecular rotation restriction induced by the aptamer upon binding of adenosine. The optimal component ratio of the probe was AIE molecule/DNA aptamer = 100 (μM/μM). The calibration curve of adenosine detection showed a linear range of 10 pM to 0.5 μM with an R2 of 0.996, and the detection limit of the probe was 10 pM. The probe exhibited a good selectivity to adenosine against its analogs (uridine, guanosine, and cytidine). The probe was used to detect adenosine in urine samples, a recovery from 86.8% to 90.0% for the spiked concentrations of adenosine (0.01, 0.05, 0.1 μM). The relative standard deviation from 1.2% to 2.0% was obtained. The intra-day and inter-day tests also showed good precisions, with measurement RSD values of 2.3% and 2.1%, respectively.

Quantification of 16 β-lactams in chicken muscle by QuEChERS extraction and UPLC-Q-Orbitrap-MS with parallel reaction monitoring

A method is described for the analysis of 16 β-lactams in chicken muscle by UPLC-quadrupole(Q)-Orbitrap-MS with parallel reaction monitoring (PRM). QuEChERS approach includes clean-up step by sorbent of primary-secondary amine (PSA) and C18 was adopted for sample preparation. Q-Orbitrap with PRM showed high sensitivity with limits of detection (LODs) ranged from 0.01μgkg−1 to 0.35μgkg−1. The method was further validated by intra- and inter-day test with spiking levels less than MRLs (maximum residue limits, the European Union). Recovery (83–112%) and precision values (RSDs <15%) for all studied analytes were obtained. The result indicates that UPLC-Q-Orbitrap coupled with QuEChERS preparation can serve as a routine quantification method for β-lactam residues in chicken muscles.

Selective pre and post blast trinitrotoluene detection with a novel ethylenediamine entrapped thin polymer film and digital image colorimetry

A novel test kit was developed for the selective detection of trinitrotoluene (TNT). A thin film of ethylenediamine (EDA)-entrapped polyvinyl chloride was fabricated within a small tube which made the kit easily portable. A red-brown complex was obtained from a selective reaction of released EDA with TNT. The test kit was used in conjunction with digital image colorimetry for rapid quantitative analysis of TNT. The Red-Green-Blue (RGB) values from digital photos of the colorimetric products were used as the analytical data to establish calibration curves of TNT. A wide linear range (0–100mgL−1) with good linearity (R2>0.99) and low limit of detection (1.00±0.02mgL−1–5.4±0.3mgL−1) was obtained for quantification of TNT. Good precision was obtained in both intra- and inter-day tests (2.18–5.59%RSD and 4.00–8.83%RSD, respectively). The method showed good accuracy with control and spiked soil samples: TNT readings were 8.0–12.2mgL−1 with 10mgL−1 known concentration. The test kit could be stored in both desiccator and freezer for 2 months (only +0.6% and +5.0% change in the blue channel intensity). The test kit was able to detect trace residues of TNT from an actual bombing crime scene (Ratchaprasong intersection, Bangkok) one week after the bombing.

Separation of cucurbitane triterpenoids from bitter melon drinks and determination of partition coefficients using vortex-assisted dispersive liquid-phase microextraction followed by UHPLC analysis.

A rapid, effective method applying vortex-assisted liquid-liquid microextraction before ultra-high performance liquid chromatography with mass spectrometry and evaporative light scattering detection was developed for the analysis of four cucurbitane triterpenoids (momordicoside L, momordicoside K, momordicoside F2 , and 3β,7β,25-trihydroxy cucurbita-5,23(E)-dien-19-al) in bitter melon juices. Variables affecting the extraction efficiency including different extraction solvents, volume of extraction solvent, salt amount, acid condition, vortex speed and time were optimized thoroughly. Under the optimum conditions, precision was determined by the intra- and inter-day tests in a range of 1.1-5.7% and 2.9-4.0% (RSD), respectively, with recoveries between 95.7 and 106.1%. The calibration curves showed good linearity with square correlation coefficient of 0.9936-0.9991 (evaporative light scattering detection) and 0.9858-0.9989 (MS). The detection limits ranged from 0.8-1.9ng/mL (MS) to 3-10ng/mL (evaporative light scattering detection) for these compounds. Enrichment factors of four target compounds were between 27 and 63 times. The proposed method was also used to determine the apparent solvent/water partition coefficients of analytes within the range of 53-120. The developed method can effectively enrich and quantify cucurbitane triterpenoids from bitter melon drinks.

Simultaneous determination of four compounds, campesterol, emodin8-O-β-D-Glucopyranoside, quercetin, and isoquercitrin in Reynoutria sachalinensis by high-performance liquid chromatography-diode array detector

Background:Reynoutria sachalinensis is a well-known and used herbal medicine to treatment of arthralgia, jaundice, amenorrhea, coughs, carbuncles, and sores.Objective:We have developed high-performance liquid chromatography analysis method for simultaneous determination of isolated four compounds, campesterol, emodin8-O-β-D-glucopyranoside, quercetin, and isoquercitrin from R. sachalinensis is.Materials and Methods:The four compounds were separated on Shiseido C18 column (S-5 μm, 4.6 mm I.D. ×250 mm) at a column temperature of 25°C. The mobile phase composed of water and methanol with gradient elution system, and flow rate is 1.0 ml/min. The detection wavelength was set at 205 nm.Results:Validation of this analytical method was evaluated by linearity, precision, and accuracy test. This established method had good linearity (R2 > 0.997). The relative standard deviation values of intra- and inter-day testing were indicated that <2%, and accuracy is 91.66%–103.31% at intraday and 91.69%–103.31% at intraday. The results of recovery test were 92.60%–108.99%.Conclusion:In these results, developed method was accurate and reliable to the quality evaluation of campesterol, emodin 8-O-β-D-glucopyranoside, quercetin, and isoquercitrin isolated from R. sachalinensis.SUMMARY We have developed high-performance liquid analysis method for simultaneous determination of 4 compounds of Reynoutria sachalinensis. Abbreviations used: HPLC: High-performance liquid chromatography, DAD: Diode array detector, LOD: Limit of detection, LOQ: Limit of quantitation, ICH: International Conference on Harmonisation.

Quantitative detection of sulfadimethoxine in fish based on the recognition of gold nanoparticles labeled aptamers

Gold nanoparticles ( Aunps) have been investigated as novel marking materials for their unique luminescent properties.Aptamer is a type of recognition materials with specific binding ability to capture target molecules and have been widely applied in the field of analysis and detection. In our study, a novel detection method for quantitative analysis of sulfadimethoxine was developed based on Au NPs and aptamer.The proposed method was applied to the analysis of real samples.The recoveries were 85.64% and 89.86%, and the relative standard deviation ( RSD) values were 4.00%, 5.28%, and 5.88%, 6.67%, for intra-and inter-day tests, respectively.The linear range of the method was 110 ng/m L, and the detection limit was1 ng/m L.The above results suggested that the proposed method was highly accurate, and precise, and was feasible for the quantification of target sulfadimethoxine in aquatic product.

Rapid determination of six carcinogenic primary aromatic amines in mainstream cigarette smoke by two-dimensional online solid phase extraction combined with liquid chromatography tandem mass spectrometry

A fully automated, rapid, and reliable method for simultaneous determination of six carcinogenic primary aromatic amines (AAs), including o-toluidine (o-TOL), 2, 6-dimethylaniline (2, 6-DMA), o-anisidine (o-ASD), 1-naphthylamine (1-ANP), 2-naphthylamine (2-ANP), and 4-aminobiphenyl (4-ABP), in mainstream cigarette smoke was established. The proposed method was based on two-dimensional online solid phase extraction combined with liquid chromatography tandem mass spectrometry (SPE/LC–MS/MS). The particulate phase of the mainstream cigarette smoke was collected on a Cambridge filter pad and pretreated via ultrasonic extraction with 2% formic acid (FA), while the gas phase was trapped by 2% FA without pretreatment for determination. The two-dimensional online SPE comprised of two cartridges with different absorption characteristics was applied for sample pretreatment. Analysis was performed by liquid chromatography coupled with tandem mass spectrometry (LC–MS/MS) under multiple reaction monitoring mode. Each sample required about 0.5h for solid phase extraction and analysis. The limit of detections (LODs) for six AAs ranged from 0.04 to 0.58ng/cig and recoveries were within 84.5%–122.9%. The relative standard deviations of intra- and inter-day tests for 3R4F reference cigarette were less than 6% and 7%, respectively, while no more than 7% and 8% separately for a type of Virginia cigarette. The proposed method enabled minimum sample pretreatment, full automation, and high throughput with high selectivity, sensitivity, and accuracy. As a part of the validation procedure, fifteen brands of cigarettes were tested by the designed method.

The intra-rater reliability of a revised 3-point grading system for accessory joint mobilizations

Objectives: Joint mobilizations are often quantified using a 4-point grading system based on the physiotherapist’s detection of resistance. It is suggested that the initial resistance to joint mobilizations is imperceptible to physiotherapists, but that at some point through range becomes perceptible, a point termed R1. Grades of mobilization traditionally hinge around this concept and are performed either before or after R1. Physiotherapists, however, show poor reliability in applying grades of mobilization. The definition of R1 is ambiguous and dependent on the skills of the individual physiotherapist. The aim of this study is to test a revised grading system where R1 is considered at the beginning of range, and the entire range, as perceived by the physiotherapists maximum force application, is divided into three, creating 3 grades of mobilization.Method: Thirty-two post-registration physiotherapists and nineteen pre-registration students assessed end of range (point R2) and then applied 3 grades of AP mobilizations, over the talus, in an asymptomatic models ankle. Vertical forces were recorded through a force platform. Intra-class Correlation Coefficients, Standard Error of Measurement, and Minimal Detectable Change were calculated to explore intra-rater reliability on intra-day and inter-day testing. T-tests determined group differences.Results: Intra-rater reliability was excellent for intra-day testing (ICC 0.96–0.97), and inter-day testing (ICC 0.85–0.93). No statistical difference was found between pre- and post-registration groups.Discussion: Standardizing the definition of grades of mobilization, by moving R1 to the beginning of range and separating grades into thirds, results in excellent intra-rater reliability on intra-day and inter-day tests.Level of Evidence: 3b.

Simultaneous characterization and quantification of 17 main compounds in Rabdosia rubescens by high performance liquid chromatography

Rabdosia rubescens is a healthy herbal tea and well-known Chinese medicinal herb. To evaluate the quality of R. rubescens from China, a high performance liquid chromatography method with dual-wavelength detection was developed and validated. The method was successfully applied for the simultaneous characterization and quantification of 17 main constituents from four different cultivation regions in China. Under optimal conditions, analysis was performed on a Luna C-18 column and gradient elution with a solvent system of acetonitrile and 0.5% (v/v) acetic acid–water at a flow rate of 1.0 mL/min and wavelength of 220 nm and 280 nm. All standard calibration curves exhibited good linearity (r2 > 0.9992) within the test ranges. The precision was evaluated by intraday and interday tests, which revealed relative standard deviation values within the ranges of 0.57–2.35% and 0.52–3.40%, respectively. The recoveries were in the range of 96.37–101.66%. The relative standard deviation values for stability and repeatability were < 5%. The contents of some compounds were low and varied with different cultivars. The proposed method could serve as a prerequisite for quality control of R. rubescens materials and products.

Validity and reliability of a simple ‘low-tech’ test for measuring choice stepping reaction time in older people

Objective: To establish the psychometric properties of a simple ‘low-tech’ choice stepping reaction time test (CSRT-M) by investigating its validity and test–retest reliability. Design: Cross-sectional. Setting: Community. Subjects: A total of 169 older people from the control arm of a clinical trial and a convenience sample of 30 older people. Main measures: Demographic, physical, cognitive and prospective falls data were collected in addition to CSRT-M. The CSRT-M time was taken as the total time to complete 20 steps onto four targets printed on a portable rubber mat. Assessment of the original electronic version (CSRT-E) and re-administration of the CSRT-M the next day was done in 30 participants. Results: Multivariate regression analysis showed that the CSRT-M time was best explained by leaning balance control, quadriceps strength and cognitive functioning (R2 = 0.44). Performance on the CSRT-M was worse in older participants and participants with a presence of fall risk factors, supporting good discriminant validity. The odds of suffering multiple future falls increased by 74% (odds ratio (OR) = 1.74, 95% CI (confidence interval) = 1.14–2.65, p = 0.010) for each standard deviation increase in CSRT-M, supporting good predictive validity. Criterion validity was confirmed by a strong bivariate correlation between CSRT-M and CSRT-E (0.81, p < 0.001). Test–retest reliability for the CSRT-M was good (intraclass correlation coefficient = 0.74, 95% CI = 0.45–0.88, p < 0.001). Conclusions: A simple test of unplanned volitional stepping (CSRT-M) has excellent predictive validity for future falls, good inter-day test–retest reliability and excellent criterion validity with respect to the well-validated CSRT-E. The CSRT-M, therefore, may be a useful fall risk screening tool for older people.