• Title/Summary/Keyword: liquid standard

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Comparison of Efficacy in Abnormal Cervical Cell Detection between Liquid-based Cytology and Conventional Cytology

  • Tanabodee, Jitraporn;Thepsuwan, Kitisak;Karalak, Anant;Laoaree, Orawan;Krachang, Anong;Manmatt, Kittipong;Anontwatanawong, Nualpan
    • Asian Pacific Journal of Cancer Prevention
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    • v.16 no.16
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    • pp.7381-7384
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    • 2015
  • This study was conducted to 1206 women who had cervical cancer screening at Chonburi Cancer Hospital. The spilt-sample study aimed to compare the efficacy of abnormal cervical cells detection between liquid-based cytology (LBC) and conventional cytology (CC). The collection of cervical cells was performed by broom and directly smeared on a glass slide for CC then the rest of specimen was prepared for LBC. All slides were evaluated and classified by The Bethesda System. The results of the two cytological tests were compared to the gold standard. The LBC smear significantly decreased inflammatory cell and thick smear on slides. These two techniques were not difference in detection rate of abnormal cytology and had high cytological diagnostic agreement of 95.7%. The histologic diagnosis of cervical tissue was used as the gold standard in 103 cases. Sensitivity, specificity, positive predictive value, negative predictive value, false positive, false negative and accuracy of LBC at ASC-US cut off were 81.4, 75.0, 70.0, 84.9, 25.0, 18.6 and 77.7%, respectively. CC had higher false positive and false negative than LBC. LBC had shown higher sensitivity, specificity, PPV, NPV and accuracy than CC but no statistical significance. In conclusion, LBC method can improve specimen quality, more sensitive, specific and accurate at ASC-US cut off and as effective as CC in detecting cervical epithelial cell abnormalities.

Comparison of Anthocyanin Content in Seed Coats of Black Soybean [Glycine max(L.) Merr.] Cultivars Using Liquid Chromatography Coupled to Tandem Mass Spectrometry

  • Shin, Sung-Chul;Lee, Soo-Jung;Lee, Sung-Joong;Chung, Jong-Il;Bae, Dong-Won;Kim, Soo-Taek;Sung, Nak-Ju
    • Food Science and Biotechnology
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    • v.18 no.6
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    • pp.1470-1475
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    • 2009
  • The seed coat of the black soybean contains 3 main anthocyanins such as delphinidin-3-O-$\beta$-glucoside, cyanidin-3-O-$\beta$-glucoside, and petunidin-3-O-$\beta$-glucoside. As a part of our effort on discovering and breeding new black soybean cultivars which possesses specific anthocyanin component rich, we determined the anthocyanin profiles of the 2 cultivars recently developed soybean cv. Gaechuck #1 and cv. Gyeongsang #1, using liquid chromatography-tandem mass spectrometry (LC-MS/MS) and compared their content and identity with those of previously known 10 cultivar controls. The Cosmosil-$5C_{18}$-AR-II column were selected for the analysis because of the best peak separation. The column temperature was set up at $35^{\circ}C$. The mobile phase consisting of water containing 0.5%(v/v) formic acid and methanol gave good separation between the 3 anthocyanin analytes and internal standard (quercetin 3-O-$\beta$-rutinoside) and peaks with suppressed tail. The MS/MS spectra of each individual anthocyanin standard were detected in positive electron spray ionization (ESI) modes. It was disclosed that the anthocyanin contents of the soybean cv. Gaechuck#1 and cv. Gyeongsang#1 are roughly higher than those of the 10 controls.

Rapid identification and toxin type analysis of Clostridium perfringens isolated from healthy or diseased stocks with necrotic enteritis in chichen (닭의 괴사성 장염 및 건강 계군에서 분리한 Clostridium perfringens의 신속동정 및 독소형 분석)

  • Kim, Hong-jib;Kang, Mun-il;Chung, Un-ik
    • Korean Journal of Veterinary Research
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    • v.37 no.1
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    • pp.137-146
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    • 1997
  • About Clostridium perfringens causing clinically necrotic enteritis or isolated from the intestinal contens of healthy chicken, We examined the usefulness of a rapid identification method by gas-liquid chromatography as well as the types of toxins. For this study, there were used 169 chickens including 116 broilers, 27 layers and 26 breeders which collected from 9 healty flock and 21 diseased flock showing necrotic enteritis. Among them, Cl perfringens was isolated from 30 chickens(17.8%) including 7 breeders(26.9%), 5 layers(18.5%) and 18 broilers(15.5%). Isolation of Cl perfringens was mainly from ceca (100%) and followed by small intestines(70.0%) and livers(16.7%), respectively. Average concentration of the pathogen in intestinal contents was $10^{3.8}CFU/g$ in cases occuring necrotic enteritis and on the contrary $10^{3.8}CFU/g$ in healthy cases. All isolates tested showed the same characterstics in biochemical tests compared to those in standard strain. Analysis of gas-liquid chromatography to volatile fatty acids produced by Cl perfringens in PYG broth showed the typical peaks of acetic and butyric acids compatible with the standard chromogram and was confirmed as a effective and reliable tool for rapid identification of the bacteria. Toxin types of 30 strains were mostly classified in A type(26 isolates) and the rest in C type(2 isolates) and unidentifed type(2 isolates). All the isolates were highly susceptible to amphicillin, amoxicillin and cephalothin.

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Verification of Analytical Method of Azaspiracid Toxins in Shellfish and Tunicates by Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS (Liquid Chromatography-Tandem Mass Spectrometry)를 이용한 패류 및 피낭류 중 아자스필산 분석법의 유효성 검증)

  • Cho, Sung Rae;Jeong, Sang Hyeon;Park, Kunbawui;Yoon, Minchul;Kim, Dong Wook;Son, Kwang Tae;Ha, Kwang Soo
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.54 no.4
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    • pp.404-410
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    • 2021
  • Although, mouse bioassay for the monitoring of azaspiracids (AZAs) toxins in shellfish has been used previously, the reported method has low sensitivity and it is time-consuming. Recently, there is an interest in the quantitative analysis of AZAs using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The purpose of this study is to verify the simultaneous analysis of AZAs in shellfish and tunicate in Korea using LC-MS/MS. To validate the method, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, accuracy, and repeatability were determined. All standard compounds were analyzed within 7 min. The correlation coefficients (R2) of the standard solution was higher than 0.9995 (within the range of 0.8-10.0 ㎍/L). The LODs and LOQs of AZAs in shellfish were 0.08-0.16 ㎍/kg and 0.23-0.50 ㎍/kg, respectively. The accuracy and precision of the method for determining AZAs in shellfish were 87.1-93.0% and 1.23-4.91%, respectively. Consequently, the verified LC-MS/MS method is suitable to analyze AZAs in shellfish and tunicates in Korea.

Development of a Sensitive Analytical Method of Polynemoraline C Using LC-MS/MS and Its Application to a Pharmacokinetic Study in Mice

  • Pang, Minyeong;Lee, Jaehyeok;Jeon, Ji-Hyeon;Song, Im-Sook;Han, Young Taek;Choi, Min-Koo
    • Mass Spectrometry Letters
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    • v.12 no.4
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    • pp.200-205
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    • 2021
  • Polynemoraline C, a pyridocoumarin alkaloid, exhibits anticholinergic, anti-inflammatory, antitumor, and antimicrobial activities. A sensitive analytical method of polynemoraline C in mouse plasma was developed and validated using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Polynemoraline C and 13C-caffeine (internal standard) in mouse plasma were extracted using a liquid-liquid extraction method coupled with ethyl acetate. This extraction method resulted in high and reproducible extraction recovery in the range of 73.49%-77.31% with no interfering peaks around the peak retention time of polynemoraline C and 13C-caffeine. The standard calibration curves for polynemoraline C were linear over the range of 0.5-200 ng/mL with r2 > 0.985. The accuracy, precision, and the stability of the data were within acceptable limits on the FDA guideline. After intravenous and oral administration of polynemoraline C at doses of 5 and 30 mg/kg, respectively, the present method was successfully applied to the pharmacokinetic study of polynemoraline C. Polynemoraline C in mouse plasma showed a multi-exponential elimination pattern with a high volume of distribution values. This compound's absolute oral bioavailability was found to be 17.0%. Polynemoraline C's newly developed LC-MS/MS method can be used for further studies on the efficacy, toxicity, and biopharmaceutics of polynemoraline C, as well as its pharmacokinetic studies.

Experimental Study of Droplet Characteristics Related to Electrospray Mode (정전분무모드에 관한 액적특성의 실험적 연구)

  • Kim, Ji Yeop;Lee, Doe Hyun;Cho, Ju Hyung;Hong, Jung Goo
    • Journal of ILASS-Korea
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    • v.27 no.1
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    • pp.26-35
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    • 2022
  • Electrospray is a method of atomizing fluid using high voltage supply and capable of generating continuous flow and coherent size of droplets. Electrical system and properties of fluids has enabled electrospray to have various spray modes. However, its studies have been confined only in Cone jet, which is more stable and easier to manipulate droplets' size than other spraying modes. Therefore, it is necessary to investigate and compare other spraying modes based on experimental parameters and physical properties of fluids. This research paper identified nine different spray modes. It was found out that Sauter Mean Diameter (SMD) is proportional to flow rate of fluids and maximum difference among spray modes was 1.7 times. On the other hand, SMD standard deviation had low variations on specific flow rates of fluids. Pulsed jet mode recorded the largest SMD standard deviation, while Spindle recorded the lowest.

Determination of Tiapride in Human Plasma Using Hydrophilic Interaction Liquid Chromatography-Tandem Mass Spectrometry

  • Moon, Ya;Paek, In-Bok;Kim, Hui-Hyun;Ji, Hye-Young;Lee, Hye-Won;Park, Hyoung-Geun;Lee, Hye-Suk
    • Archives of Pharmacal Research
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    • v.27 no.9
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    • pp.901-905
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    • 2004
  • A rapid, sensitive and selective hydrophilic interaction liquid chromatography-tandem mass spectrometric(HILIC-MS/MS) method for the determination of tiapride in human plasma was developed. Tiapride and internal standard, metoclopramide were extracted from human plasma with dichloromethane at basic pH and analyzed on an Atlantis HILIC silica column with the mobile phase of acetonitrile-ammonium formate (190 mM, pH 3.0) (94:6, v/v). The ana-Iytes were detected using an electrospray ionization tandem mass spectrometry in the multi-ple-reaction-monitoring mode. The standard curve was linear (r=0.999) over the concentration range of 1.00-200 ng/mL. The coefficient of variation and relative error for intra- and inter-assay at three QC levels were 6.4∼8.8% and -2.0∼3.6%, respectively. The recoveries of tiapride ranged from 96.3 to 97.4%, with that of metoclopramide (internal standard) being 94.2%. The lower limit of quantification for tiapride was 1.00 ng/mL using 1 00 $\mu$L of plasma sample.

Development of Isotope Dilution LC-MS/MS Method for Accurate Determination of Arsenobetaine in Oyster Certified Reference Material

  • Lee, Woo Young;Yim, Yong-Hyeon;Hwang, Euijin;Lim, Youngran;Kim, Tae Kyu;Lee, Kyoung-Seok
    • Bulletin of the Korean Chemical Society
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    • v.35 no.3
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    • pp.821-827
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    • 2014
  • An isotope dilution liquid chromatography tandem mass spectrometry (ID LC-MS/MS) method has been developed and applied to the determination of arsenobetaine (AsB, ${(CH_3)_3}^+AsCH_2COO^-$) from oyster candidate certified reference material (CRM). The exact matching isotope dilution approach was adopted for accurate determination of AsB using $^{13}C_2$-labeled AsB as an internal standard. Efficiencies of different AsB extraction methods were evaluated using a codfish reference material and a simple sonication method was selected as the method of choice for the certification of the oyster candidate CRM. The hydrophilic interaction liquid chromatography (HILIC) combined with electrospray ionization tandem mass spectrometry (ESI/MS/MS) in selected reaction monitoring (SRM) mode was optimized for adequate chromatographic retention and robust quantification of AsB from codfish and oyster samples. By analyzing 12 subsamples taken from each 12 bottles systematically selected from the whole oyster CRM batch, the certified value of AsB was determined as $6.60mg{\cdot}kg^{-1}{\pm}0.31mg{\cdot}kg^{-1}$ and it showed excellent between-bottle homogeneity of less than 0.42%, which is represented by relative standard deviation of 12 bottles from the CRM batch. The major source of uncertainty was the certified value of the AsB standard solution.

A Study on the Concentration of Aflatoxin B1 in Granule and Globular Types of Herbal Medicines (엑스과립과 환으로 만들어진 한방생약제제의 aflatoxin B1 연구)

  • Bae, Jong-Sup;Kim, Yong-Ung;Park, Moon-Ki
    • Journal of Environmental Science International
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    • v.19 no.2
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    • pp.209-215
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    • 2010
  • This study is an endeavor to evaluate the risk assessment of hazardous(aflatoxin $B_1$) in medicines from oriental medical prescription which are circulated much recently. For that, twelve globular and granule types, seven liquid types of herbal medicine were bought to compare and analyze the content of aflatoxin aflatoxin B_1), which are harmful to human body. Woo Hwang Cheong Sim Hwan of Aflatoxin $B_1$ concentration lower than the standard accepted by all the products have been detected, B company(tradition) is the concentration of $1.24\;{\mu}g/kg$, C company $1.04\;{\mu}g/kg$, A company(tradition) and B company did not detect. And the general pill of aflatoxin B1 concentration lower than the standard accepted by all the products have been detected, S-1 is the concentration of $1.8\;{\mu}g/kg$, S-2 of $1.04\;{\mu}g/kg$, S-3 of $0.88\;{\mu}g/kg$, S-4 of $9.32\l\;{\mu}g/kg$, S-6 of $7.8\;{\mu}g/kg$, S-5 did not detect. All the products eundan allowed in the concentration of aflatoxin $B_1$ levels were lower than detection, D company of $0.96\;{\mu}g/kg$, E company concentration was not detected. The liquid product of aflatoxin $B_1$ concentration was found liwer than the standard accepted by all the product, L-3 concentration of $0.8\;{\mu}g/kg$, K-4 was detected in the $1.16\;{\mu}g/kg$, L-1 and L-2 is not detected, L-5 concentration of $15\;{\mu}g/kg$, L-7 is detected as $1.08\;{\mu}g/kg$ and, L-6 was not detected.

A Study on the Simultaneous Determination of Residual Zeranol, Zearalenone and Their Metabolites in Beef by Gas Chromatography/Mass Spectrometry (Gas Chromatography/Mass Spectrometry에 의한 우육 중의 잔류 Zeranol, Zearalenone 및 그 대사산물들의 동시 분석법에 대한 연구)

  • 이은섭;이용욱
    • Journal of Food Hygiene and Safety
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    • v.9 no.1
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    • pp.1-13
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    • 1994
  • A Simultaneous determination method was improved for the determination and confirmation of zeranol, zearalenone, as well as their isomers and metabolites, in beef. The analytes were extracted from tissue by CH3CN, hydrolyzed enzymatically(for glucuronide conjugates), cleaned up by a strong basic anion exchange resin combined with a liquid/liquid partitioning, derivatized using MSTFA and confirmed, quantified by GC/MS/SIM with a internal standard, zearalane. The results were as follows : (1) all the estrogens were separated on the GC/MS chromatogram under the extraction method and the chromatographic conditions improved, the retention times of zearalane-TMS2, zearalanone-TMS2, zearalenone-TMS2, zeranol-TMS3, taleranol-TMS3, and $\alpha$-zearalenol-TMS3, $\beta$-zearalenol-TMS3, were 18.49, 19.44, 19.63, 19.71, 19.79 and 19.99, 20.08 minutes, respectively. (2) The calibration curves of residual zeranol, zearalenone and their metabolites showed constantly linear(r=0.99) in the range of 5~20 ng. The minimum detection concentration of residual zeranol, zearalenone and their metabolites was 1 ppb. (3) The total average recovery of residual zeranol, zearalenone and their metabolites from spiked beef was 60.2%(CV=29.7%) at the 1 ppb and 63.5%(CV=26.5) at the 2 ppb, 72.9%(CV=18.2%) at the 4 ppb. (4) The preservation method for 6 estrogens was improved for the fast running time(21 min) and MSTFA was utilized for derivatizing 6 estrogens for improvement of recovery, for good resolution, for characteristic mass spectra unlike Jose's method and Tina's method. The utilization of zearalane as internal standard showed good quantification result for zeranol, zearalenone, as well as their isomers and metabolites, in beef.

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