• Title, Summary, Keyword: HPLC-MS/MS

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Analytical Characteristics of GC/MS and HPLC according to the Concentration Distribution of PAHs (PAHs 농도 분포에 따른 GC/MS와 HPLC의 분석특성에 관한 연구)

  • Hong, Jwa-Ryung;Choi, Kwang-Min
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.25 no.3
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    • pp.312-321
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    • 2015
  • Objectives: The purpose of this study was to determine the best method to analyze PAHs at extremely low concentrations. To this end, 16 PAHswere analyzed simultaneously by GC/MS, HPLC/FLD and HPLC/UVD, and the analytical characteristics of HPLC and GC/MS were compared. Methods: This study was conducted by GC/MS and HPLC/FLD/UVD, and evaluated linearity, precision and detection limit. Standard solutions were prepared for 21 samples in the range of $0.00001{\sim}1.0{\mu}g/mL$ and the samples were divided into four groups. All samples were made in three sets and analysis was replicated seven times. Results: Sixteen PAHs could be simultaneously separated by HPLC and GC/MS, and the adequate equipment was HPLC/FLD. The retention times by HPLC were shorter than GC/MS, and HPLC had better separation for most PAHs than GC/MS. The peaks of naphthalene and naphthalene-D8 partially overlapped for GC/MS. HPLC/FLD had a 20-2000 times lower limit of detection than GC/MS and UVD. However FLD was not adequate for analyzing acenaphthylene because it has too low a fluorescence quantum yield to be detected. The precision of HPLC/FLD/UVD and GC/MS showed less than 20% at $0.001{\mu}g/mL$ PAHs and when the concentration was higher, the coefficient of variation was decreased. HPLC/FLD was better for the overall detection of limits. Conclusions: The results indicate that the HPLC/FLD method has good linear range, precision and a detection of limits from $0.00001{\sim}0.0001{\mu}g/mL$ for all 16 PAHs. This study contributes to providing useful data for analysis technology and can be applied to occupational exposure measurement for PAHs in workplaces.

Analysis of Marker Substances in Samul-tang by HPLC-MS/MS (HPLC-MS/MS에 의한 사물탕의 지표성분 분석)

  • Yu, Young-Beob;Kim, Mi-Jung;Huang, Dae-Sun;Ha, Hye-Kyeong;Ma, Jin-Yeul;Shin, Hyeun-Kyoo
    • The Korea Journal of Herbology
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    • v.22 no.2
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    • pp.97-102
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    • 2007
  • Objectives : This study presents a high performance liquid chromatography - electrospray ionization-mass spectrometer (HPLC-MS/MS) methods for the quantitative and qualitative analysis of various active components in Samul-tang, which is composed of four crude herbs. Methods : HPLC-ESI-MS/MS for the determinations of paeoniflorin and 5-HMF (5-hydroxymethyl 2-furaldehyde) in the Samul-tang, the separation method was performed on an COSMOS1L 5C18-AR-Il (2.0 X 150 mm I.D.) column by gradient elution with 0.1% acetic acid and 5% CH3CN in water (A)-0.1% acetic acid and 5% H20 in CH3CN (B) as the mobile phase at a flow-rate of 300 ${\mu}L/min$ with detection at quadrupole mass spectrometer. The all marker substances were always detected as the base peaks in the positive ion mode. Results : The paeoniflorin of Paeoniae Radix in Samul-tang showed a strong base peak [M+H2O]+ in the positive detection mode to give the following as; paeoniflorin (498.109 [M+H2O]+, 479.8 [M]+, 301 [M-glucose]+, 179.3 [glucose]+). Based on the HPLC retnetion time and MS of standard compounds confirmed the identity of active compounds in Rehmanniae Radix Preparata as follows; 5-HMF (127.0[M+H]+, 109.3 [M-OH]+) in the positive ion mode. Conclusion : According to the above results, HPLC-ESI-MS method permits assignment of tentative structures such as paeoniflorin and 5-HMF in the Samul-tang.

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Multiresidue Analysis of 240 Pesticides in Apple and Lettuce by QuEChERS Sample Preparation and HPLC-MS/MS Analysis (QuEChERS 전처리법과 HPLC-MS/MS 기기분석을 이용한 사과와 상추 중 240종 농약의 동시분석)

  • Kwon, Hye-Young;Kim, Chan-Sub;Park, Byung-Jun;Jin, Yong-Duk;Son, Kyung-Ae;Hong, Su-Myeong;Lee, Je-Bong;Im, Geon-Jae
    • The Korean Journal of Pesticide Science
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    • v.15 no.4
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    • pp.417-433
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    • 2011
  • The study tested QuEChERS (quick, easy, cheap, effective, rugged and safe) sample preparation and HPLC-MS/ MS analysis for measurement of pesticide residues in fruit and vegetable. 240 kinds of pesticides spiked at three levels of 90, 45, 9 ng/g in lettuce and apple. For QuEChERS sample preparation, graphitized carbon black (GCB) was used for only lettuce in dispersive-SPE as absorbent. Matrix-matched standard calibration was used for quantitative analysis of HPLC-MS/MS. 218 pesticides (91%) in apple and 207 pesticides (86%) in lettuce showed recoveries in the range of 70~120% with $RSD{\leq}20%$. The lowest calibrated level (LCL) were 4.5 ng/g for 192 pesticides, 9 ng/g for 42 pesticides, 45 ng/g for 3 pesticides and 3 pesticides were not detected at all concentration levels. The results showed that the QuEChERS sample preparation and HPLC-MS/MS analysis can be applied to multi-residue analysis of pesticides in vegetables and fruits.

Effects of Herbal Medicine on Breastfeeding - Analysis of Marker Substances in Saenghwa-tang by HPLC and LC/MS/MS - (산모의 한약 복용이 모유에 미치는 영향 - HPLC와 LC/MS/MS를 이용한 생화탕 지표성분 분석 -)

  • Park, Ka-Young;Lee, Ah-Young;Ban, Ji-Hye;Park, Jung-Kyung;Lee, Eun-Hee
    • The Journal of Korean Obstetrics and Gynecology
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    • v.26 no.4
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    • pp.48-65
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    • 2013
  • Objectives: We took breast milk samples and analyzed them using HPLC and LC/MS/MS, to evaluate the effects of taking Saenghwa-tang during breastfeeding on breast milk. Methods: The study participants were 20 lactating women who admitted in Korean medical postpartum care center. Breast milks were collected from paticipants who have been administrated Saenghwa-tang for more than 3 days. We used HPLC and LC/MS/MS for the determinations of amygdalin, liquiritins, 6-gingerol, decursin and decursinol angelate in Saenghwa-tang. Results: 1. Participants' $Mean{\pm}S.D$ (standard deviation) of age is $31.05{\pm}1.96$, and 15 participants had normal delivery and 5 participants had cesarean delivery. 12 participants were primipara and 8 participants were multipara. $Mean{\pm}S.D$ of lactating date is $9.4{\pm}0.94$. 2. Using HPLC, we learned LOQ level peak that matches the peak retention time of standard components of Saenghwa-tang was not detected from 20 breast milk samples. 3. Using LC/MS/MS, decursin of Angelicae Gigantis Radix was detected from HMSP 02, HMSP 04, HMSP 06, HMSP 11, and the each concentrations are 16, 2, 64, 11 ppb. Liquiritin of Glycyrrhizae Radix was not detected from HMSP 13~HMSP 18. Conclusions: Data obtained by this approach shows that this method is reliable and suitable for determining the safety of taking Saenghwa-tang during breastfeeding.

Structural determination of triterpenic acids in Prunellae Spica by fast atom bombardment tandem mass spectrometry (하고초의 생리활성 성분 Triterpenic Acids의 FAB-MS를 이용한 구조 규명)

  • Ahn, Young Min;Lee, Kang Ro;Hong, Jongki
    • Analytical Science and Technology
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    • v.21 no.4
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    • pp.245-258
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    • 2008
  • Five triterpenic acids as marker compounds were extracted and isolated from Prunellae Spica by column chromatography and reversed-phase high-performance liquid chromatography (HPLC), and their purity was determinated by HPLC (purity ${\geq}90%$). Molecular weight and elemental compositions of the five marker compounds were determined by fast atom bombardment high-resolution mass spectrometry (FAB-HRMS). The structural determination of the five marker compounds was carried out fast atom bombardment collision-induced dissociation tandem mass spectrometry (FAB-CID-MS/MS). The collision-induced dissociation (CID) of protonated molecules $[M+H]^+$ and deprotonated molecules $[M-H]^-$ produced diverse product ions due mainly to retro Diels-Alder reaction (RDA), dehydration and decarboxylation. Moreover, the CID-MS/MS spectra of the $[M-H]^-$ ions were observed charge-remote fragmentation (CRF) patterns. On the basis of interpretation of CID-MS/MS spectra, structural elucidation of triterpenic acids isolated from Prunellae Spica was clearly performed.

Determination of 11 Illicit Compounds in Dietary Supplements Using High-Performance Liquid Chromatography and Liquid Chromatography-Tandem Mass Spectrometry

  • Shin, Dasom;Kang, Hui-Seung;Kim, Hyung-soo;Moon, Guiim
    • Journal of Food Hygiene and Safety
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    • v.35 no.4
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    • pp.326-333
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    • 2020
  • In this work, we developed an analytical method for determining 11 illicit compounds in dietary supplements using high-performance liquid chromatography and liquid chromatography-tandem mass spectrometry. Eleven target compounds, including those meant for weight loss (7-keto-dihydroepiandrosterone, buformin, metformin, phenformin, salbutamol, and tolbutamide), sexual enhancement (dihydroepiandrosterone), and relaxation (asarone, kavain, magnoflorine, and picamilon) were screened and confirmed in dietary supplements. Method validation was performed by evaluating the selectivity, linearity, limit of quantification (LOQ), accuracy, and precision according to the Association of Official Analytical Chemists guidelines. The linearity was > 0.993 for all analytes. The LOQs were ranged in 2.1-9.9 ㎍/mL (HPLC-DAD) and 0.002-0.008 ㎍/mL (LC-MS/MS). The accuracies (expressed as recovery) were 90.0-106% (HPLC-DAD) and 83.0-114% (LC-MS/MS). The precision (expressed as the relative standard deviation) was below 10% using HPLC and LC-MS/MS. The proposed method can be used for the surveillance of illicit compounds in dietary supplements.

Analysis of Microcystins(LR, YR and RR) in Water (Micro-HPLC/IS/MS에 의한 수 중의 Microcystins (LR, YR 및 RR)의 분석)

  • Park, Kwan Su;Bae, Jun Hyun;Kang, Jun Gil;Kim, Youn Doo
    • Journal of the Korean Chemical Society
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    • v.45 no.6
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    • pp.524-531
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    • 2001
  • Micro-HPLC/IS/MS after solid phase extraction has been employed to enhance the accu-racy in the determination of toxic microcystins, such as microcystin-LR, -YR and -RR. The absorbance at 238 nm in HPLC/UV and characteristic spectra of 135 m/z and $[M+H]^+$ m/z in MS have been widely monitored to identify those microcystin-LR, -YR and -RR. In this study, new lines at 507 m/z for LR, 520 m/z for RR and 532 m/z for YR have been additionally detected in the micro-HPLC/IS/MS spectrum, corresponding to double charge. The micro-HPLC/IS/MS methodology has been applied to investigate the presence of the toxic microcystins in Taecheong lake.

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Comparison of Methods for Measuring Histamine by ELISA and HPLC-MS Assay In Vitro (In Vitro에서 히스타민 측정 시 ELISA법과 HPLC-MS 분석법의 비교)

  • Lee, In Hee;Kim, Yoo Hyun
    • Korean Journal of Clinical Laboratory Science
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    • v.47 no.4
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    • pp.306-312
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    • 2015
  • The measurement of histamine is to determine the degree of allergy because the allergic reaction can lead to the release of histamine. In general, the antigen-antibody reaction was quantified by measuring absorbance using a microplate reader. In this study, we compare the method using a general antigen-antibody reaction and the method using a high performance liquid chromatography mass spectrometer (HPLC-MS) of chemical analysis in the measurement of histamine secretion. The cell line used was RBL-2H3, an allergic reaction was induced by stimulation with C48/80 (compound 48/80). Allergy-induced cells degranulation rate was confirmed by measurement of ${\beta}$-hexosaminidase and cytotoxicity was performed for the validity of the experiment. The quantitative determination of histamine showed a significant difference, since the quantitative limit of the measurement by the antigen-antibody reaction was 10.257 ppm while the quantitative limit of the measurement by HPLC-MS was 0.020 ppm. Measurement of histamine in allergic activity and anti-allergy tests showed that the HPLC-MS analysis rather than the analysis of the antigen-antibody reaction is a more precise and accurate test.

Quantification of Momilactones A and B in Rice Straw

  • Lee, Choon-Woo;Koichi Yoneyama;Yasutomo Takeuchi;Ryu, Su-Noh
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.47 no.4
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    • pp.283-285
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    • 2002
  • Momilactones A and B, the major phytotoxins and phytoalexins in rice plants, were quantified by a HPLC-APCI-MS-MS (APCI-MS-MS) system under multiple reaction monitoring conditions. Since MA and MB were found to be easily extracted with water, these phytotoxic compounds may affect germination and growth of other plant species when the rice straws were left in the fields.

Effective Analysis of Dicyclanil in Lamb and Chicken Muscle using HPLCUV/Vis and LC/MS/MS

  • Kim, Byung-Ju;Myung, Seung-Woon
    • Mass Spectrometry Letters
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    • v.2 no.2
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    • pp.45-48
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    • 2011
  • The authors describe a method for monitoring dicyclanil levels in lamb and chicken muscle tissues. The devised procedure involves dicyclanyl extraction by SPE and its detection HPLC-UV/Vis and LC/MS/MS. The method was found to have LOD and LOQ values of $0.02\;mg\;kg^{-1}$ and $0.05\sim0.06\;mg\;kg^{-1}$, respectively. The intraday precision and an accuracy of spiked samples were found to have 2.3~10.4 RSD% and 80.9~105.7%, respectively.