• Archives of Pharmacal Research
• /
• v.27 no.12
• /
• pp.1202-1206
• /
• 2004

A rapid, sensitive and selective liquid chromatography-tandem mass spectrometric (LC-MS/ MS) method for the determination of lithospermic acid B (LSB) in rat serum was developed. LSB and internal standard, 7-hydroxy-3-phenyl-chromen-4-one (HPC) were extracted from rat serum with methyl-tert-butyl ether at acidic pH and analyzed on a Luna $C_8$ column with the mobile phase of acetonitrile-ammonium formate (10 mM, pH 6.5) (50:50, v/v). The analytes were detected using a negative electrospray ionization tandem mass spectrometry in the multiple- reaction-monitoring mode. The standard curve was linear $(r^2 = 0.997)$ over the concentration range of 10.0-500 ng/mL. The coefficient of variation and relative error for intra- and interassay at three QC levels were 1.1~6.2% and -10.3~-2.7%, respectively. The recovery of LSB from serum sample ranged from 73.2 to 79.5%, with that of HPC (internal standard) being 75.1 %. The lower limit of quantification for LSB was 10 ng/mL using 50 ${\mu}L$ of serum sample.

• Analytical Science and Technology
• /
• v.14 no.6
• /
• pp.471-475
• /
• 2001

Solid phase microextraction(SPME) with $85{\mu}m$-polyacrylate (PA) and $100{\mu}m$-polydimethylsiloxane(PDMS) fibers, coupled to gas chromatography-mass spectrometry was used to determine 1,2-dibromo-3-chloropropane(DBCP) and n-butylbenzene in water. The conditions affecting the SPME process(i.e, extraction time, injection length, injection temperature, desorption time and temperature) were optimized. The linearity of the calibration curve (correlation coefficient, R) was over 0.99 and the limits of detection of the method were between 1.5 and $10.8{\mu}g/L$. Repeatability of the method was between 10.4 and 14.4 %.

• Nuclear Engineering and Technology
• /
• v.51 no.2
• /
• pp.533-538
• /
• 2019

The mechanical-collimation imaging is the most mature technology in prompt gamma (PG) imaging which is considered the most promising technology for beam range verification in proton therapy. The purpose of the present study is to compare the performances of two mechanical-collimation PG cameras, knife-edge (KE) camera and multi-slit (MS) camera. For this, the PG cameras were modeled by Geant4 Monte Carlo code, and the performances of the cameras were compared for imaginary point and line sources and for proton beams incident on a cylindrical PMMA phantom. From the simulation results, the KE camera was found to show higher counting efficiency than the MS camera, being able to estimate the beam range even for $10^7$ protons. Our results, however, confirmed that in order to estimate the beam range correctly, the KE camera should be aligned, at least approximately, to the location of the proton beam range. The MS camera was found to show lower efficiency, being able to estimate the beam range correctly only when the number of the protons is at least $10^8$. For enough number of protons, however, the MS camera estimated the beam range correctly, errors being less than 1.2 mm, regardless of the location of the camera.

• Journal of Food Hygiene and Safety
• /
• v.31 no.5
• /
• pp.327-334
• /
• 2016

This study was conducted to establish the standard method for the contents of biotin in milk formulas. To optimize the method, we compared several conditions for liquid extraction, purification and instrumental measurement using spiked samples and certified reference material (NIST SRM 1849a) as test materials. LC-MS/MS method for biotin was established using $C_{18}$ column and binary gradient 0.1% formic acid/acetonitrile, 0.1% formic acid/water mobile phase is applied for biotin. Product-ion traces at m/z 245.1 ${\rightarrow}$ 227.1, 166.1 are used for quantitative analysis of biotin. The linearity was over $R^2=0.999$ in range of $5{\sim}60{\mu}g/L$. For purification, chloroform was used as a solvent for eliminating lipids in milk formula. The linearity was over 0.999 in range of 5~60 ng/mL. The detection limit and quantification limit were 0.10, 0.31 ng/mL. The accuracy and precision of LC-MS/MS method using CRM were 103%, 2.5% respectively. Optimized methods were applied in sample analysis to verify the reliability. All the tested milk formulas were acceptable contents of biotin compared with component specification and standards for nutrition labeling. The standard operating procedures were prepared for biotin to provide experimental information and to strengthen the management of nutrient in milk formula.

• Advances in concrete construction
• /
• v.11 no.3
• /
• pp.207-217
• /
• 2021

This study relates to a production of Quaternary Cement Concrete (QCC) prepared by using Micro Silica (MS), Marble Dust (MD) and Rice Husk Ash (RHA), followed by an investigation towards fresh and hardened properties of blended concrete. A total of 39 mixes were cast by incorporating different percentages of MS (6%, 7% and 8%), MD (5%, 10% and 15%) and RHA (5%, 10%, 15% and 20%) as partial replacement of Ordinary Portland Cement. The workability of fresh concrete was maintained in the range of 100±25 mm by adding 0.7% of Super Plasticizer in the mix. Optimum mechanical strength was observed at combination of 8% MS+5% MD+10% RHA. Marble dust replacement from 10 to 15% and Rice husk ash replacements from 15 to 20% depicted a substantial reduction in compressive strength at all ages. Durability parameter with respect to water absorption at 28 days shows an increasing trend as the percentage of blending increases.

• Analytical Science and Technology
• /
• v.31 no.4
• /
• pp.161-170
• /
• 2018

The epidemic of disorders associated with synthetic stimulants, such as methamphetamine (MA) and amphetamine (AP), is a health, social, legal, and financial problem. Owing to the high potential of their abuse and addiction, reliable analytical methods are required to detect and identify MA, AP, and their metabolites in biological samples. Thus, a dilute-and-shoot liquid chromatography-tandem mass spectrophotometry (LC-MS/MS) was developed for simultaneous determination of MA, 4-hydroxymethamphetamine (4HMA), AP, and 4-hydroxyamphetamine (4HA) in urine. Urine sample ($100{\mu}L$) was mixed with $50{\mu}L$ of mobile phase consisting of 0.4 % formic acid and methanol and $50{\mu}L$ of working internal-standard solution. Aliquots of $8{\mu}L$ diluted urine was injected into the LC-MS/MS system. For all analytes, chromatographic separation was performed using a C18 reversed-phase column with gradient elution and a total run time of 5 min. The identification and quantification were performed by multiple reaction monitoring (MRM). Linear least-squares regression was conducted to generate a calibration curve, with $1/x^2$ as the weighting factor. The linear ranges were 2.0-200, 1.0-800, and 10-2500 ng/mL for 4HA and 4HMA, AP, and MA, respectively. The inter- and intraday precisions were within 6.6 %, whereas the inter- and intraday accuracies ranged from -14.9 to 11.3 %. The low limits of quantification were 2.0 ng/mL (4HA and 4HMA), 1.0 ng/mL (AP), and 10 ng/mL (MA). The proposed method exhibited satisfactory selectivity, dilution integrity, matrix effect, and stability, which are required for validation. Moreover, the purification efficiency of high-speed centrifugation was clearly higher than 6-15 % for QC samples (n=5), which was higher than that of the membrane-filtration method. The applicability of the proposed method was tested by forensic analysis of urine samples from drug abusers.

• Analytical Science and Technology
• /
• v.18 no.4
• /
• pp.320-328
• /
• 2005

The most common five chlorophenols (4-chloro-3-methylphenol, 2,4,5-trichlorophenol, 2,4,6-trichlorophenol, 2,3,4,6-tetrachlorophenol, pentachlorophenol) were determined from the industrial wastewater by GC/MS. The samples were collected from the petrochemical company, textile company and leather making company. The developed analytical method was modified by USEPA Method 3510. The samples were extracted with dichloromethane under pH 2 and pH 5-6, and determined by the GC/MS with SIM mode. There were good linearities (above $R^2=0.9943$) on e ranges of the 0.1 ng/mL~10 ng/mL and 0.5 ng/mL~10 ng/mL, and the limit of detection were between 0.1 ng/mL and 0.5 ng/mL. The absolute recoveries were measured at the concentration of 1, 5, and 10 ng/mL, and the recovery was 71.6~98.9% except for PCP. The relative standard deviation (RSD) was 1.2~14.3% and it gave a good reproducibility for the assay. The bias, which shows the accuracy, was a good although it was a little high values (11.3~22.1%) at the low concentration (1 ng/mL).

• Analytical Science and Technology
• /
• v.29 no.1
• /
• pp.29-34
• /
• 2016

This study explores the means by which MX can be effectively extracted from chlorinated water 3-Chloro-4-(dichloromethyl)-5-hydroxy-2(5H)-furanone (MX), a potent mutagen commonly found in chlorinated drinking water at concentrations of up to a few hundred ng/L, was quantitatively determined using sample enrichment followed by liquid-liquid extraction (LLE), derivatization to methylated form, and analysis with GC-MS. A 4-L water sample was enriched to a concentration of 0.4 L using a vacuum rotary evaporator at 30 ℃. MX in the water was extracted using ethyl acetate (100 mL × 2) as a solvent and MX in the extract was methylated with 10 % H₂SO₄ in methanol. MX was recovered at a rate of 73.8 %, which was higher than that (38.1 %) for the resin adsorption method. The limit of quantification and repeatability (as relative standard deviation) were estimated to be 10 ng/L and 2.2 %, respectively. This result suggested that LLE can be used for the determination of MX in chlorinated water as an alternative to more time-consuming resin adsorption method.

• Biomolecules & Therapeutics
• /
• v.15 no.4
• /
• pp.266-272
• /
• 2007

A rapid analytical method was developed to quantify very long-chain fatty acids (VLCFAs, C22:0, C24:0, C26:0) in human plasma with good sensitivity and specificity using tert-butyldimethylsilyl (TBDMS) derivatization and stable isotope GC-MS selective ion monitoring (GC-MS/SIM). Two-hundred and fifty ${\mu}L$ of plasma was fortified with deuterated stable isotope internal standards (d3-C22:0, d3-C24:0, d3-C26:0) and standard mixtures of chloroform and methanol, and then extracted with hexane and acetonitrile. To upper layer of liquid-liquid-extraction, N-(t-Butyldimethylsilyl)-N-methyltrifluoroacetamide was added and then heated to $60^{\circ}C$ for 30 min to produce the TBDMS derivatives. Derivatives of VLCFAs were analyzed by GC-MS/SIM. Calibration curves showed a linear relationship for the target compounds in the concentration range of $10^{-4}{\sim}2{\times}10^3\;{\mu}g/mL$ with the correlation coefficient ranging from 0.996 to 0.999. The limit of quantification for the plasma was $10^{-4}{\sim}2{\times}10^{-4}\;{\mu}g/mL$ (S/N=3). When applied to the plasma specimens of patients with peroxisomal disorder, X-linked adrenoleucodystropy (ALD, Mckusick 202370), the method clearly differentiated normal subjects from ALD patients. The C24:0/C22:0 and C26:0/C22:0 ratios were significantly elevated in the plasma of patients with X-linked ALD compared to normal subjects. The new developed method might be useful for a rapid and sensitive diagnosis of X-linked ALD and other peroxisomal disorders.

• Applied Biological Chemistry
• /
• v.39 no.6
• /
• pp.517-520
• /
• 1996

To identify the volatiles of Platycodon roots, the three-year-old and the 24-year-old Platycodon roots cultivated in a local farm were extracted with ethyl ether by SDE method. 54.71mg% and 80.01mg% of volatile components were collected in the three-year-old and in 24-year-old Platycodon roots, respectively. As a result of GC/MS(TIC) analysis, 24 and 28 compounds were identified, respectively; The amounts of volatile components such as hexanol, trans-2-hexenol and nonanal in 24-year-old roots were detected above ten times than those in 3-year-old roots. The Volatiles of 24-year-old roots were fractionated by SCC and identified by GC/MS to be 10 hydrocarbons, 8 alcohols, 10 aldehydes, 5 esters, 6 acids and 1 unknown compound as the major components. The species and total amounts of volatile component in 24-year-old Platycodon roots were considered to be higher than those in 3-year-old Platycodon roots. *Abbreviations 1. Platycodon : platycodon grandiflorus (jacquin) A. De Candolle. 2. SDE : Simultaneous Distillation Extraction 3. SCC : Silicagel Column Chromatography 4. GC : gas chromatography 5. GC/MS : Gas Chromatography-Mass Spectrometer 6. TIC : Total Ion Chromatogoraphy