• Analytical Science and Technology
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• v.8 no.4
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• pp.771-778
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• 1995

The authors have developed an analytical method for determining trace amounts of 285 kinds of chemicals in natural waters by GC-ion trap MS. The results of overall recovery tests at $0.1{\mu}g/l$ showed that the mean recovery was 92.1% and the mean relative standard deviation was 10.8%. The mean of the method detection limits was $0.036{\mu}g/l$. From the results of analysis of real samples, it was confirmed that this method is useful to elucidate the concentration levels and the fate of chemicals in the aquatic environment.

• Bulletin of the Korean Chemical Society
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• v.32 no.4
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• pp.1170-1178
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• 2011

In the present study, the approach of high accuracy mass measurements for phospholipid identifications was evaluated using a 7 T ESI-FTMS/linear ion trap MS/MS. Experiments were carried out for porcine brain, bovine liver, and soybean total lipid extracts in both positive and negative ion modes. In total, 59, 55, and 18 phospholipid species were characterized in the positive ion mode for porcine brain, bovine liver, and soybean lipid extracts, respectively. Assigned lipid classes were PC, PE, PEt, PS, and SM. In the negative ion mode, PG, PS, PA, PE, and PI classes were observed. In the negative ion mode, for porcine brain, bovine liver, and soybean lipid extracts, 28, 34, and 29 species were characterized, respectively. Comparison of our results with those obtained by other groups using derivatization-LC-APCI MS and nano-RP-LC-MS/MS showed that our approach can characterize PC species as effectively as those methods could. In conclusion, we demonstrated that high accuracy mass measurements of total lipid extracts using a high resolution FTMS, particularly, 7T FTMS, plus ion-trap MS/MS are very useful in profiling lipid compositions in biological samples.

• Mass Spectrometry Letters
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• v.5 no.1
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• pp.24-29
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• 2014

An advanced and reliable high performance liquid chromatography (HPLC)/ultraviolet detector (UV)/ion-trap time-of-flight (IT-TOF) mass spectrometry was developed for the simultaneous quantification of 19 marker compounds in Bang-poong-tong-sung-san (BPTS), a traditional oriental prescription. Various parameters affecting HPLC separation and IT-TOF detection were investigated, and optimized conditions were identified. The separation was achieved on a Capcell PAK C18 column ($1.5mm{\times}250mm$, $5{\mu}m$ particle size) using a gradient elution of acetonitrile and water containing 0.1% formic acid at a flow rate of 0.1 mL/min. The column temperature was maintained at $40^{\circ}C$ and the injection volume was $2{\mu}L$. IT-TOF system was equipped with an electrospray ion source (ESI) operating in positive or negative ion mode. The optimized electrospray ionization parameters were as follows: ion spray voltage, +4.5 kV (positive ion mode), or -3.5 kV (negative ion mode); drying gas ($N_2$), 1.5 L/min; heat block temperature, $200^{\circ}C$. Automatic $MS^n$ (n = 1~3) analyses were carried out to obtain structural information of analytes. Elemental compositions and their mass errors were calculated based on their accurate masses obtained from a formula predictor software. The marker compounds in BPTS were identified by comparisons between $MS^n$ spectra from standards and those from extracts. Moreover, the libraries of $MS^2$ and $MS^3$ spectra and accurate masses of parent and fragment ions for marker compounds were constructed. The developed method was successfully applied to the BPTS extracts and identified 17 out of 19 marker compounds in the BPTS extracts.

• Archives of Pharmacal Research
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• v.28 no.10
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• pp.1190-1195
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• 2005

The objective of this study was to develop an assay for mequitazine (MQZ) for the study of the bioavailability of the drug in human subjects. Using one mL of human plasma, the pH of the sample was adjusted and MQZ in the aqueous phase extracted with hexane; the organic layer was then evaporated to dryness, reconstituted and an aliquot introduced to a gas chromatograph/mass spectrometer (GC/MS) system with ion-trap detector. Inter- and intra-day precision of the assay were less than 15.1 and $17.7{\%}$, respectively; Inter- and intra-day accuracy were less than 8.91 and $18.6{\%}$, respectively. The limit of quantification for the current assay was set at 1 ng/mL. To determine whether the current assay is applicable in a pharmacokinetic study for MQZ in human, oral formulation containing 10 mg MQZ was administered to healthy male subjects and blood samples collected. The current assay was able to quantify MQZ levels in most of the samples. The maximum concentration ($C_{max}$ was 8.5 ng/mL, which was obtained at 10.1 h, with mean half-life of approximately 45.5 h. Under the current sampling protocol, the ratio of $AUC_{t{\rightarrow}last}$ to $AUC_{t{\rightarrow}{\infty}}$ was $934{\%}$, indicating that the blood collection time of 216 h is reasonable for MQZ. Therefore, these observations indicate that an assay for MQZ in human plasma is developed by using GC/MS with ion-trap detector and validated for the study of pharmacokinetics of single oral dose of 10 mg MQZ, and that the current study design for the bioavailability study is adequate for the drug.

• Bulletin of the Korean Chemical Society
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• v.23 no.8
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• pp.1097-1102
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• 2002

The mass spectrometry using an ion trap tandem mass spectrometer has been investigated to find optimum conditions for the analysis of benzo(a)pyrene (3,4-benzpyrene). The applicability to a real soil sample was also investigated to verify the usef ulness of the MS/MS (or collision induced dissociation, CID) analysis. The optimum CID condition was 1.5 and 0.45 for the RF excitation voltage and the q value, respectively. For comparison, CID and EI were applied to the analysis of a soil sample. CID analysis was more sensitive than EI analysis of the soil sample. The limit of detection (LOD) of benzo(a)pyrene was 3.18 ng mL-1 and 0.85 ng mL,-1 for EI and MS/MS analysis, respectively. The precision at the soil sample for EI and CID showed relative standard deviations of 6.1% and 4.1%, respectively, and the concentrations were 168 ㎍ kg-1 and 162 ㎍ kg-1 , respectively.

• Analytical Science and Technology
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• v.15 no.1
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• pp.7-14
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• 2002

Laser ablation ion trap mass spectrometry (LAITMS) was developed for the analysis of metal and ceramic samples. For this study, XeCl excimer laser (308 nm) was used for ablating the samples and ITMS was used as a detector. Samples were introduced from outside of a ring electrode and this way of sample introduction was very effective for solid samples when laser ablation was employed. Helium gas was used as a buffer gas, and its effect on sensitivity and some parameters (buffer gas pressure, ion storage time, and cut-off RF voltage) were studied. The optimized conditions were $1{\times}10^{-4}$ Torr of buffer gas pressure, 100 ms of ion storage time and $1150V_{p-p}$ of cut-off RF voltage. From that results, copper (Cu) and molybdenum (Mo) metals were tested with LAITMS and the mass spectra of these pure metals were compared with the natural abundance of isotope ratio. We also examined ceramic samples ($Al_2O_3$, $ZrO_2$) and represented the result of elemental analysis.

• Journal of Pharmaceutical Investigation
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• v.36 no.2
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• pp.123-129
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• 2006

A method determining the plasma concentration of clotiazepam was developed by using gas chromatography/mass spectrometry with an ion-trap detector and was validated for applying pharmacokinetics to human volunteers orally taken 5 mg dose of clotiazepam. The detection limit was 1 ng/ml and the limit of quantitation was 5 ng/mt. Intraday reproducibility and accuracy bias % were less than 8.2 and 10.2% with inter-day variations for those being within 7.0 and 13.8%, respectively. The recovery of clotiazepam was higher than 87%. The principal pharmacokinetic parameters were determined from the plasma concentration-time plot by non-compartmental or two-compartmental analysis. In non-compartmental analysis, the elimination half-life of 10.4 hr and the area under the curve of 651.3 ng hr/ml were determined, and the maximal concentration (158.6 ng/ml) in the plasma was obtained at 0.56 hr post-dose. The developed method can be appropriate to apply pharmacokinetics and bioequivalence of clotiazepam.

• Korean Journal of Pharmacognosy
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• v.33 no.2 s.129
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• pp.88-91
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• 2002

Liquid-chromatography coupled with electrospray-ion trap mass spectrometry was applied to the analysis of the eleutherosides B and E in the Eleutherococcus senticosus cortexes. The optimum ESI/MS results were obtained in the positive ion mode using extracted ion chromatogram targeting Na-adduct molecular ion of each compound. This method allowed rapid and simple gradient separation of underivatized eleutherosides B and E without pre-purification steps at very low concentration.

• Bulletin of the Korean Chemical Society
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• v.29 no.10
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• pp.1973-1976
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• 2008

Electronic photodepletion spectrum of dibenzo-18-crown-6 with a potassium ion ($K^+$-DB18C6) was obtained in the gas phase using electrospray ionization and quadrupole ion-trap reflectron time-of-flight mass spectrometry. The spectrum exhibited rather a broad absorption band at 36350 $cm^{-1}$, which was tentatively assigned as the origin of the S1 band. The photodepletion spectrum of $Cs^+$-DB18C6 was also obtained to elaborate the effects of metal cations on electronic and geometric structures of metal cation-DB18C6 complexes. We found that the S1 band of $Cs^+$-DB18C6 was red-shifted by 180 $cm^{-1}$ from that of $K^+$-DB18C6. With the results of quantum theoretical calculations using the density functional theory, we suggested that the red-shift arose mainly from weaker binding of $Cs^+$ to DB18C6 than that of K+, which resulted from a larger size of $Cs^+$ than that of the cavity in DB18C6.

• Progress in Medical Physics
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• v.5 no.2
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• pp.3-12
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• 1994

$\^$137/Cs gamma ray induced thermoluminescenc(TL) from Na$\^$+/ ion implanted Al$_2$O$_3$ and unimplanted Al$_2$O$_3$ and the TL from Na$\^$+/ ion implanted Al$_2$O$_3$ are measured over the temperature range of 340K～620K. The TL curve of Na$\^$+/ ion implanted Al$_2$O$_3$ induced by $\^$137/Cs gamma ray is split into iolated TL peak located at 415K, 452K, 508K, and 568K. Because that the concentration of trapped char he carries of $\^$137/Cs gamma ray induced Al$_2$O$_3$ implanted with Na$\^$+/ ion is larger than that of Na$\^$+/ ion only implanted Al$_2$O$_3$, and the trap concentration of Na$\^$+/ ion implanted Al$_2$O$_3$ is much than that of $\^$137/Cs gamma ray only irradiated Al$_2$O$_3$, the TL intensity of Na$\^$+/ ion implanted Al$_2$O$_3$ induced by $\^$137/Cs gamma ray is about 20 times and 5 times higher than that of Al$_2$O$_3$ only implanted with Na$\^$+/ ion and Al$_2$O$_3$ only irradiated with $\^$137/Cs gamma ray, respectively. In proportion as ion implantation does and energy are incresed, the number of generated defects and the rate of defect creation are incresed, respectively. Therefore the TL intensity of ion implanted Al$_2$O$_3$ is depend on ion dose and energy. Acccrding to increse of incident ion mass, the TL intensity of ion implanted Al$_2$O$_3$ is abruptly decresce. This result showes that the TL intensity of ion implanted Al$_2$O$_3$ is closely related to ion depth range as wll as rate of defect creatin. The TL intensity of ion implanted Al$_2$O$_3$ is found to be related with defects generated by ion implantation. Table Caption