• 제목/요약/키워드: simultaneous recovery

검색결과 315건 처리시간 0.035초

Simultaneous Quantitative Determination of Nine Hallucinogenic NBOMe Derivatives in Human Plasma Using Liquid Chromatography Tandem Mass Spectrometry

  • Seo, Hyewon;Yoo, Hye Hyun;Kim, Young-Hoon;Hong, Jin;Sheen, Yhun Yhong
    • Mass Spectrometry Letters
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    • 제10권1호
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    • pp.18-26
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    • 2019
  • We developed a bioanalytical method for simultaneous determination of nine NBOMe derivatives (25H-NBOMe, 25B-NBOMe, 25E-NBOMe, 25N-NBOMe, 25C-NBOH, 25I-NBOH, 25B-NBF, 25C-NBF, and 25I-NBF) in human plasma using liquid chromatography tandem mass spectrometry (LC-MS/MS). Human plasma samples were pre-treated using solid-phase extraction. Separation was achieved on a C18 column under gradient elution using a mobile phase containing 0.1% formic acid in acetonitrile and 0.1% formic acid in water at a flow rate of 0.3 mL/min. Mass detection was performed in the positive ion mode using multiple reaction monitoring. The calibration range was 1-100 ng/mL for all quantitative analytes, with a correlation coefficient greater than 0.99. The intra- and inter-day precision and accuracy varied from 0.85 to 6.92% and from 90.19 to 108.69%, respectively. The recovery ranged from 86.36 to 118.52%, and the matrix effects ranged from 27.09 to 99.72%. The stability was acceptable in various conditions. The LC-MS/MS method was validated for linearity, accuracy, precision, matrix effects, recovery and stability in accordance with the FDA guidance. The proposed method is suitable for reliable and robust routine screening and analysis of nine NBOMe derivatives in forensic field.

Development of a Simultaneous Analytical Method for Diquat, Paraquat and Chlormequat in Animal Products Using UPLC-MS/MS

  • Cho, Il Kyu;Rahman, Md. Musfiqur;Seol, Jae Ung;Noh, Hyun Ho;Jo, Hyeong-Wook;Moon, Joon-Kwan
    • 한국환경농학회지
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    • 제39권4호
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    • pp.368-374
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    • 2020
  • BACKGROUND: The residual analysis of polar pesticides has remained a challenge. It is even more difficult to simultaneously analyze multiple polar pesticides. Diquat, paraquat, and chlormequat are typical examples of highly polar pesticides. The existing methods for the analysis of diquat, paraquat and chlormequat are complex and time consuming. Therefore, a simple, quick and effective method was developed in the represent study for simultaneous analysis of diquat, paraquat and chlormequat in animal products, meat and fat using UPLC-MS/MS. METHODS AND RESULTS: Sample extraction was carried out using acidified acetonitrile and water and re- extracted with acidified acetonitrile and combine the extracts followed by centrifugation. The extract was then cleaned up with a HLB cartridge after reconstitution with acidic acetonitrile and water. The method was validated in quintuplicate at three different concentrations. The limits of detection (LOD) and quantification (LOQ) were 0.0015 and 0.005 mg/L, respectively. Matrix suppression effect was observed for all of the analytes. A seven point matrix matched calibration curve was constructed for each of the compound resulted excellent linearity with determination coefficients (R2) ≥ 0.991. Accuracy and precision of the method was calculated from the recovery and repeatability and ranged from 62.4 to 119.7% with relative standard deviation less than 18.8%. CONCLUSION: The recovery and repeatability of the developed method were in the acceptable range according to the Codex Alimentarius guideline. The developed method can be applied for the routine monitoring of diquat, paraquat, and chlormequat in animal products, meat and fat.

Clinical Features and Hearing Outcomes of Sudden Sensorineural Hearing Loss in Diabetic Patients

  • Ju, Yeo Rim;Park, Hyoung-sik;Lee, Min Young;Jung, Jae Yun;Choi, Ji Eun
    • Journal of Audiology & Otology
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    • 제25권1호
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    • pp.27-35
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    • 2021
  • Background and Objectives: This study aimed to evaluate the clinical features and the clinical factors associated with prognosis of sudden sensorineural hearing loss (SSNHL) in diabetic patients. Subjects and Methods: Forty-nine diabetic with unilateral SSNHL were retrospectively included. All patients received systemic high dose steroid therapy within one month after onset and had more than one month of follow-up audiogram. The basic characteristics of the patients, initial and follow-up audiograms, laboratory data, and methods of steroid treatment were collected. Results: Compared to reference values in healthy subjects, 79%, 55%, and 45% of the patients had higher values of mean neutrophil-lymphocyte ratio (NLR), platelet-lymphocyte ratio (PLR), and lymphocyte-monocyte ratio (LMR), respectively. Older patients had significantly less degree of hearing loss, but they also had significantly worse hearing thresholds in the unaffected ear. After steroid treatment, less than half patients (47%) showed hearing recovery. Simultaneous intratympanic dexamethasone (ITD) injections with systemic steroid did not confer an additional hearing gain or an earlier recovery rate in diabetic patients with SSNHL. In the multivariate analysis, initial hearing thresholds of affected ear and timing of steroid treatment were significantly associated with hearing prognosis in diabetic patients with SSNHL. Conclusions: Diabetic patients with SSNHL tended to have increased NLR, LMR, and PLR, which are reported to be associated with microvascular angiopathy. Simultaneous ITD injections to improve hearing recovery in diabetic patients with SSNHL seems unnecessary.

Clinical Features and Hearing Outcomes of Sudden Sensorineural Hearing Loss in Diabetic Patients

  • Ju, Yeo Rim;Park, Hyoung-sik;Lee, Min Young;Jung, Jae Yun;Choi, Ji Eun
    • 대한청각학회지
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    • 제25권1호
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    • pp.27-35
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    • 2021
  • Background and Objectives: This study aimed to evaluate the clinical features and the clinical factors associated with prognosis of sudden sensorineural hearing loss (SSNHL) in diabetic patients. Subjects and Methods: Forty-nine diabetic with unilateral SSNHL were retrospectively included. All patients received systemic high dose steroid therapy within one month after onset and had more than one month of follow-up audiogram. The basic characteristics of the patients, initial and follow-up audiograms, laboratory data, and methods of steroid treatment were collected. Results: Compared to reference values in healthy subjects, 79%, 55%, and 45% of the patients had higher values of mean neutrophil-lymphocyte ratio (NLR), platelet-lymphocyte ratio (PLR), and lymphocyte-monocyte ratio (LMR), respectively. Older patients had significantly less degree of hearing loss, but they also had significantly worse hearing thresholds in the unaffected ear. After steroid treatment, less than half patients (47%) showed hearing recovery. Simultaneous intratympanic dexamethasone (ITD) injections with systemic steroid did not confer an additional hearing gain or an earlier recovery rate in diabetic patients with SSNHL. In the multivariate analysis, initial hearing thresholds of affected ear and timing of steroid treatment were significantly associated with hearing prognosis in diabetic patients with SSNHL. Conclusions: Diabetic patients with SSNHL tended to have increased NLR, LMR, and PLR, which are reported to be associated with microvascular angiopathy. Simultaneous ITD injections to improve hearing recovery in diabetic patients with SSNHL seems unnecessary.

역상소형컬럼 전처리를 이용한 Ginsenoside의 신속정량법 (A Rapid Method of Ginsenoside Analysis in HPLC by Pretreatment through the reverse-phase minicolumn)

  • 이미경;임선욱;박훈
    • Journal of Ginseng Research
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    • 제12권2호
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    • pp.164-172
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    • 1988
  • 인삼사포닌 정량분석의 상법 purification과정을 역상소형 $C_18$ 컬럼 전처리로 대체할 수 있었으며, 분석시간은 1/4로 단축되었다. 이 방법을 사용하면 total ginsenoside의 회수율은 높으나 protopanaxatriol계 ginsenoside들의 회수율은 약간 낮았으며, 근중 농도 정도의 당류는 ginsenoside 회수율에 영향을 미치지 않았다. Ginsenoside 회수율의 변이계수는 상법의 경우보다 작았으며 이 방법에 사용되는 ginsenoside의 적정량은 10~15mg이었다. 역상소형컬럼방법은 건삼과 홍삼시료처리시에도 상법과 고도의 유의성을 나타냈다. 신속 역상소형컬럼 방법을 실제로 이용하기 위하여 8점의 시료를 동시에 처리하는 소형아크릴 장치를 사용하였다.

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Simultaneous Determination of Albiflorin, Cinnamaldehyde, Cinnamic Acid, Daidzin, Glycyrrhizin, Liquiritin, Paeoniflorin and Puerarin in Galgeun-tang by HPLC-PDA

  • Seo, Chang-Seob;Kim, Jung-Hoon;Shin, Hyeun-Kyoo
    • 대한한의학회지
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    • 제31권6호
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    • pp.8-15
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    • 2010
  • Objectives: We investigated to develop and validate HPLC-PDA methods for simultaneous determination of eight constituents in Galgeun-tang (GGT). Methods: Reverse-phase chromatography using a Gemini C18 column operating at $40^{\circ}C$, and photodiode array (PDA) detection at 230 nm, 254 nm, and 280 nm, were used for quantification of the eight marker components of GGT. 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. Results: Calibration curves were acquired with $r^2$ > 0.9999, and the relative standard deviation (RSD) values (%) for intra- and inter-day precision were less than 3.0%. The recovery rate of each component was in the range of 87.33-101.38%, with an RSD less than 7.0%. The contents of the eight components in GGT were 1.98-12.17 mg/g. Conclusions: The established method will be applied for the quantification of marker components in GGT.

Simultaneous Determination of Seven Compounds in Samsoeum by HPLC-PDA

  • Seo, Chang-Seob;Kim, Jung-Hoon;Huang, Dae-Sun;Shin, Hyeun-Kyoo
    • 대한한의학방제학회지
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    • 제18권1호
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    • pp.95-103
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    • 2010
  • Objectives : To develop and validate HPLC-PDA methods for simultaneous determination of seven constituents in Samsoeum(SSE). Methods : Reverse-phase chromatography using a Gemini C18 column operating at $40^{\circ}C$, and photodiode array(PDA) detection at 254 and 280 nm, were used for quantification of the seven marker components of SSE. 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. Results : Calibration curves were acquired with $r^2$>0.9997, and the relative standard deviation (RSD) values (%) for intra- and inter-day precision were less than 3.0%. The recovery rate of each compound was in the range of 100.07-112.65%, with an RSD less than 4.0%. The contents of seven compounds in SSE were 1.24-10.53 mg/g. Conclusions : The established method will be helpful to improve quality control of SSE.

A study on the analysis of artificial sweeteners in processed foods including emulsified foods by HPLC-DAD

  • Kim, Min-Hee;Lee, Do-Yeon;Ahn, Jang-Hyuk
    • 분석과학
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    • 제33권5호
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    • pp.209-214
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    • 2020
  • This study has been carried out to develop a standard method for quantifying of 3 permitted artificial sweeteners (including sodium saccharine, aspartame, acesulfame potassium) contained in foods by HPLC-DAD. A simple and rapid sample pretreatment method was used to remove fat and protein from the test solution with Carrez clearing regent precipitant know to be effective for protein and fat removal. The artificial sweeteners in the test solution purified through sample pretreatment were detected by high performance liquid chromatograph using a Reverse phase C18 column (5 ㎛, 4.6 × 250 mm). The simultaneous quantitative test of 3 kinds of artificial sweeteners can be effectively performed on the high fat emulsified foods containing a large amount of fat. Using the established simultaneous quantitative test method, artificial sweeteners were tested in foods such as dairy products, snacks and chocolate. The results calibration curve showed good linearity with high regression coefficients and the result of recovery test showed satisfactory recoveries within 80~110 %.

동시냉난방 열펌프 시스템의 운전모드별 성능특성에 관한 실험적 연구 (Experimental Study on the Performance Characteristics of a Simultaneous Heating and Cooling Heat Pump System at Each Operating Mode)

  • 강훈;이선일;주영주;정현준;김용찬;최종민
    • 설비공학논문집
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    • 제19권10호
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    • pp.679-686
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    • 2007
  • The cooling load in winter season is significant in many commercial buildings and hotels because of the usage of office equipments and the high efficiency of wall insulation. The development of a multi-heat pump that can cover heating and cooling simultaneously for each indoor unit is required. In this study, a 4-room simultaneous heating and cooling heat pump system was designed and its performance was measured at each operating mode. The system used R-410A and adopted variable speed compressor. The problems on the designed system were analyzed and defined. In addition, the solutions of the problems were suggested to improve system efficiency and to obtain the stable operation.

동시냉난방 열펌프 시스템의 운전모드별 성능특성에 관한 수치적 연구 (Numerical Study on the Performance Characteristics of a Simultaneous Heating and Cooling Heat Pump System at each Operation Mode)

  • 주영주;정현준;강훈;최종민;이무연;김용찬
    • 대한설비공학회:학술대회논문집
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    • 대한설비공학회 2007년도 동계학술발표대회 논문집
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    • pp.370-375
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    • 2007
  • The cooling load in winter season is significant in many commercial buildings and hotels because of the usage of office equipments and high efficiency of wall insulation. The development of a multi-heat pump that can cover heating and cooling simultaneously for each indoor unit is required. In this numerical study, a 4-room simultaneous heating and cooling heat pump system was modeled and its performance was calculated at each operating mode. Also, performance analysis was compared with experimental results.

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