• Title/Summary/Keyword: simultaneous recovery

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Simultaneous Determination of the Novel Neuroprotective Agent KR-31378 and its Metabolite KR-31612 Using High Performance Liquid Chromatography with Tandem Mass Spectrometry in Human Plasma

  • Kim, John;Ji, Hye-Young;Yoo, Sung-Eun;Kim, Sun-Ok;Lee, Dong-Ha;Lim, Hong;Lee, Hye-Suk
    • Archives of Pharmacal Research
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    • v.25 no.5
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    • pp.647-651
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    • 2002
  • An LC/MS/MS method for the simultaneous determination of a neuroprotective agent for ischemia-reperfusion damage, KR-31378 and its N-acetyl metabolite KR-31612 in human plasma was developed. KR-31378, KR-31612 and the internal standard. KR-31543 were extracted from human plasma by liquid-liquid extraction. A reverse-phase HPLC separation was performed on Luna phenylhexyl column with the mixture of acetonitrile-5 mM ammonium formate (55:45, v/v) as mobile phase. The detection of analytes was performed using an electrospray ionization tandem mass spectrometry in the multiple reaction monitoring mode. The lower limits of quantification for KR-31378 and KR-31612 were 2.0 ng/ml. The method showed a satisfactory sensitivity, precision, accuracy, recovery and selectivity.

Study on the development of simultaneous-rapid screening methods for residues pesticides in livestock products (수입 축산식품에서의 잔류농약 동시분석법 개발에 관한 연구)

  • Kim, Jong-shu;Kim, Gon-sup;Hah, Dae-sik
    • Korean Journal of Veterinary Research
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    • v.37 no.1
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    • pp.213-220
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    • 1997
  • A simple and rapid method known as matrix solid phase dispersion(MSPD) for simultaneous determination of 11 pesticide(2,4,5,6-tetrachlor m-xylene, ${\alpha}$-BHC, ${\gamma}$-BHC, ${\delta}$-BHC, aldrin, chlorfulazuron, heptachloroepoxide, dieldrine, endrin, endosulfan sulfate, and tetradifon) in beef fat was estabilished. Beef fat(0.5g) was fortified by adding the 11 pesticides and dibutylchlorendate as internal standard, and blended with 2g bulk $C_{18}$ in pestle and motar. Pesticides were eluted from an extraction column composed of $C_{18}$/ fat matrix blend and 2g activated Florisil by addition of 8ml acetonitrile. Then $2{\mu}l$ portion of the acetonitrile elute was directly analyzed by gaschromatography with electron capture detection. Unfortified blank control were treated similarly. Recovery rate were ranged from $83{\pm}5.4%$ to $94.2{\pm}7.6%$, intra-assay variability and inter-assay variability were ranged from 2.3% to 7.4%(n=5 for each insecticides) and from $6{\pm}1%$ to $12{\pm}3%$(n=10 for each insecticides), respectively. These results indicated that the MSPD methodology is aceptable for the extraction, determination and screening of residues 11 chroniated pesticides in beef fat.

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Simultaneous Analysis of Pesticide Priority Pollutants in Water Samples (수질 시료 중의 Pesticide Priority Pollutants 동시분석에 관한 연구)

  • Kim Kye-Young;Kim Chong-Hyeak;Lee Sueg-Geun
    • Journal of the Korean Chemical Society
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    • v.37 no.6
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    • pp.590-598
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    • 1993
  • The simultaneous analysis of samples, 16 organic pesticides in water among 129 priority pollutants listed by EPA, was performed by GC-ECD (electron capture detector) and GC/MS-SIM (selected ion monitoring). Two extraction procedures, liquid-liquid extraction (LLE) and solid-phase extraction (SPE), were studied as an extraction and concentration method. Accuracy and precision of the methods were measured by the calculation of mean recovery and mean relative standard deviation. Finally, the detection limits, the experimental limitations, and prospects were discussed.

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Simultaneous Analysis of Liquiritin and Glycyrrhizin in Sagunja-tang by HPLC-PDA (HPLC-PDA에 의한 사군자탕 중 Liquiritin과 Glycyrrhizin의 동시분석)

  • Seo, Chang-Seob;Kim, Jung-Hoon;Shin, Hyeun-Kyoo
    • Korean Journal of Pharmacognosy
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    • v.42 no.3
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    • pp.240-245
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    • 2011
  • A high-performance liquid chromatography (HPLC) method was developed for quantitative analysis of liquiritin and glycyrrhizin in Sagunja-tang (SGT, Sijunzi-tang in Chinese), a traditional Korean medicine. HPLC analysis was performed using a Gemini C18 column operating at $40^{\circ}C$, and photodiode array (PDA) detection at 254 nm and 280 nm for quantification of the two components in SGT. The mobile phase using a gradient flow consisted of two solvent systems. Solvent A was 1.0% (v/v) aqueous acetic acid and solvent B was acetonitrile with 1.0% (v/v) acetic acid. Calibration curves were acquired with $r^2$ values > 0.9998, and the relative standard deviations (RSDs, %) for intra- and inter-day precision were not exceed 4.0%. The recovery of each component was in the range of 91.85 - 108.62%, with a RSD less than 4.0%. The contents of the two components in SGT were 7.94 - 13.83 mg/g.

Simultaneous analysis of sugars by HPLC (HPLC를 이용한 당류의 동시분석법)

  • 허부홍;서형석;김성문;김영진;조종후
    • Korean Journal of Veterinary Service
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    • v.23 no.2
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    • pp.137-142
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    • 2000
  • In order to develop a good separation and simultaneous analysis of different sugar in an artificial mixed sugar solution, we analyzed 10 sugar components in an artificial mixed sugar solution composed of fructose, glucose, mannitol, sucrose, maltose, lactose, xylose, xylitol erythritol, and trehalose with using HPLC-ELSD or HPLC-RI. Separation and quantification by HPLC-ELSD was superior to those by HPLC-RI and detection sensitivity by HPLC-ELSD was higher then that by HPLC-RI as micorgram($\mu\textrm{g}$) level. 1. The units of minimal detectable limits were showed $\mu\textrm{g}$/$m\ell$ and ng/$m\ell$ by the HPLC-RI and HPLC-ELSD, respectively. 2. The condition of ELSD was drift tube temperature $82^{\circ}C$, $N_2$ gas flow rate 2.10 SLPM, and colum oven temperature $30^{\circ}C$, respectively. Isolation and recovery rates of single sugar from the multiple sugar solution was higher at the condition (time: flow rate: D.W.:ACN MeOH, min : $m\ell$/min:v:v:v) of linear gradient elution of mobile phase as 0 : 1.00 : 15 : 85 : 0.1 : 1.00 : 6 : 90 : 4, 17 : 1.00 : 10 : 70 : 20, 28 : 1.00 : 15 : 85 : 0 an 35 : 1.00 : 15 : 85 : 0, in order.

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Simultaneous Determination of Statins in Human Urine by Dilute-and-Shoot-Liquid Chromatography-Mass Spectrometry

  • Jang, Haejong;Mai, Xuan-Lan;Lee, Gunhee;Ahn, Jae Hyoung;Rhee, Jongsook;Truong, Quoc-Ky;Vinh, Dinh;Hong, Jongki;Kim, Kyeong Ho
    • Mass Spectrometry Letters
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    • v.9 no.4
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    • pp.95-99
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    • 2018
  • An innovative, simple, and rapid assay method based on liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) was developed and validated for the simultaneous determination of eight statin drugs in human urine. A simple sample clean-up procedure using the "dilute and shoot" (DAS) approach enabled a fast and reliable analysis. The influence of the dilution factor was investigated to ensure detectability and reduce the matrix effect. Chromatographic separation was performed on a Phenomenex Kinetex C18 column ($50{\times}3.0mm$ i.d., $2.6{\mu}m$) using an elution gradient of mobile phase A composed of 0.1% acetic acid, and mobile phase B composed of acetonitrile, at a flow rate of 0.35 mL/min. Quantitation was performed on a triple quadrupole mass spectrometer operated in multiple reaction monitoring (MRM) mode using electrospray ionization in positive ion mode. The total chromatographic run time was 15 min. The method was validated for selectivity, sensitivity, recovery, linearity, accuracy, precision, and stability. The present method was successfully applied to the analysis of Rosuvastatin in urine samples after oral administration to healthy human subjects.

Comparison of PET image quality using simultaneous PET/MR by attenuation correction with various MR pulse sequences

  • Park, Chan Rok;Lee, Youngjin
    • Nuclear Engineering and Technology
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    • v.51 no.6
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    • pp.1610-1615
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    • 2019
  • Positron emission tomography (PET)/magnetic resonance (MR) scanning has the advantage of less additional exposure to radiation than does PET/computed tomography (CT). In particular, MR based attenuation correction (MR AC) can greatly affect the image quality of PET and is frequently obtained using various MR sequences. Thus, the purpose of the current study was to quantitatively compare the image quality between MR non-AC (MR NAC) and MR AC in PET images with three MR sequences. Percent image uniformity (PIU), percent contrast recovery (PCR), and percent background variability (PBV) were estimated to evaluate the quality of PET images with MR AC. Based on the results of PIU, 15.2% increase in the average quality was observed for PET images with MR AC than for PET images with MR NAC. In addition, 28.6% and 71.1% improvement in the average results of PCR and PBV respectively, was observed for PET images with MR AC compared with that with MR NAC. Moreover, no significant difference was observed among the average values using three MR sequences. In conclusion, the current study demonstrated that PET with MR AC improved the image quality and can be help diagnosis in all MR sequence cases.

Validation of simultaneous mycotoxin analysis method in pet food using LC-MS/MS (LC-MS/MS를 이용한 반려동물 사료에서 곰팡이독소 동시분석법 유효성 확인)

  • Choi, Yoon Hwa;Ahn, Woo Seok;Kim, Ji Eun;Kim, Doo Hwan
    • Korean Journal of Veterinary Service
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    • v.45 no.3
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    • pp.237-242
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    • 2022
  • The simultaneous analysis of mycotoxins using LC-MS/MS, a food official analysis method, was applied with compound feed for pets with high consumer preferences. In this study, the linearity of all calibration curves showed good linearity of 0.99 or more. and both the accuracy (recovery rate) and precision (repeatability) criteria of the concentration range for each mycotoxin in the National Agricultural Products Quality Management Service's Validation and Verification Guidelines were met. And as a result of analyzing FAPAS QCM in the same way, it was assesed that the z-scores of Aflatoxin B1, Ochratoxin A, Zearalenone, and Fumonisin B1, were within ±2 range. This study showed that the application of the food official analysis method to compound feed for pets is suitable.

Simultaneous Anterior and Posterior Interosseous Nerve Syndrome Following Shoulder Arthroscopy in the Lateral Decubitus Position - Case Report - (측와위로 시행한 견관절 관절경 후에 동시에 발생한 전방 및 후방 골간 신경 증후군 - 증례보고 -)

  • Seo, Jae Sung;Kim, Jee Hoon;Kang, Dong Hwa
    • Clinics in Shoulder and Elbow
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    • v.16 no.2
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    • pp.148-152
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    • 2013
  • We report a case of simultaneous anterior and posterior interosseous nerve syndrome in association with shoulder arthroscopy. Shoulder arthroscopy was performed in a 45-year-old male patient with left shoulder instability. In the right lateral decubitus position, under general anesthesia, traction was applied with elbow extension for 2 hours. One week after surgery, the patient revisited the clinic for weakness of the flexor of the thumb, index finger, and extensor of the fingers. Recovery was not achieved after four months of observation. Therefore, nerve exploration was performed in the anterior and posterior interosseous nerve and hourglass-like fascicular constriction was detected in the posterior interosseous nerve. The area of constriction was removed and epineural neurorrhaphy was performed. Three months after exploration, the extension function of the fingers was recovered. Recovery was achieved gradually, and, five months after nerve exploration, the symptoms were completely recovered. Simultaneous anterior and posterior interosseous nerve syndrome following shoulder arthroscopy is rare. However, it could occur due to the traction and position of the patient. Thus, the operator should be careful of traction and position of the patient.

A Method for Simultaneous Analysis of Phthalate Esters and Di-(2-ethylhexyl) Adipate Migrated from PVC Wraps into Fatty Food (PVC Wraps에서 지방함유 식품으로 이행되는 Phthalate esters 및 Di-(2-ethylhexyl) adipate의 동시 분석법)

  • Lee, Kwang-Ho;Jeon, Dae-Hoon;Jeong, Dong-Youn;Choi, Byung-Hee;Kim, Sung-Wook;Lee, Chul-Won
    • Korean Journal of Food Science and Technology
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    • v.32 no.6
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    • pp.1244-1250
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    • 2000
  • A method for simultaneous quantitative determination of plasticizers such as diethyl phthalate(DEP), di-n-propyl phthalate(DprP), di-n-butyl phthalate(DBP), di-n-pentyl phthalate(DPP), butylbenzyl phthalate(BBP), di-(2-ethylhexyl) phthalate(DEHP), dicyclohexyl phthalate(DCHP) and di-(2-ethylhexyl) adipate(DEHA), which are suspected as endocrine disruptors, in food was studied. A analysis method was optimized for the quantification of plasticizers in Jjambbong, which is a kind of fatty noodle, by using GC/FID. The detection limits of DEP, DprP, DBP, DPP, BBP, DEHP, DCHP and DEHA were 3.5, 5.3, 2.2, 2.2, 7.2, 1.7, 1.9 and 3.0 mg/kg, respectively. Much higher recovery was obtained by extraction with acetone/n-hexane(1:1) rather than hexane solvent system. The recovery of DEP, DprP, DBP, DPP, BBP, DEHP, DCHP and DEHA were 72.7, 85.9, 91.4, 97.1, 100.8, 103.2, 104.3 and 95.8% after 4 time extractions, respectively. The migration of plasticizers from PVC wraps into PVC wrap covered Jjambbong was conducted after shaking(120 rpm) for 30min at room temperature with chosen solvent system. It was found that the migration level of DEHA were 577, 706, 770 mg/kg into Jjambbong, respectively, while the other plasticizers were not observed.

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