• 분석과학
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• 제8권4호
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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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• 제32권4호
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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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• 제5권1호
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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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• 제28권10호
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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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• 제23권8호
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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.

• 분석과학
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• 제15권1호
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• pp.7-14
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• 2002

본 연구에서는 레이저 애블레이션 이온 트랩 질량분석법을 이용하여 금속 및 세라믹 시료들에 대한 원소분석을 수행하였고, 이때 이온화 장치로는 XeCI 엑시머 레이저를 사용하였고 검출장치로서 이온트랩 질량 분석기를 사용하였다. 시료는 트랩의 바깥에 장착하여 시료의 교환이 매우 쉽도록 하였고 고체시료의 분석에 있어서 매우 효과적임을 밝혔다. 헬륨기체의 압력이나 이온저장시간, 초기질량제한 RF 전압 등에 대한 기초 실험을 통하여 실험의 최적 조건을 구하였고 (헬륨 기체압력 $1{\times}10^{-4}$ Torr 이온 저장시간 100 ms 초기 질량 제한전압 $1150V_{p-p}$), 이 결과를 토대로 금속시료(구리, 몰리브데늄)와 세라믹 시료(알루미나 세라믹, 지르코니아 세라믹) 들에 대한 원소분석을 수행하였다.

• Journal of Pharmaceutical Investigation
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• 제36권2호
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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.

• 생약학회지
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• 제33권2호통권129호
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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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• 제29권10호
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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.

• 한국의학물리학회지:의학물리
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• 제5권2호
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• pp.3-12
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• 1994

$Na^{+}$ 이온을 주입시킨 후, $^{17}$ Cs 감마선으로 조사된 $Al_2$O$_3$ 및, $Na^{+}$ 이 주입된 $Al_2$O$_3$의 열자극 발광을 340K～620K의 온도 구간에서 측정하였다. $Na^{+}$ 이온을 주입시킨 후, $^{137}$Cs 감마선으로 조사된 $Al_2$O$_3$의 열자극 발광 곡선은 415K, 452K, 508K, 및 568K에서 TL peak를 가지는 곡선으로 분해되었다. $Na^{+}$ 이온 주입 후 $^{137}$Cs 감마선 조사된 $Al_2$O$_3$는, $Na^{+}$ 이온만 주입된 $Al_2$O$_3$와 $^{137}$Cs 감마선 만 조사된 $Al_2$O$_3$보다 각각 defect traps에 구속된 전하운반체의 밀도와 defect traps의 밀도가 증강되었기 때문에, $Na^{+}$ 이온 주입 후 $^{137}$Cs 감마선 조사된 $Al_2$O$_3$보다 각각 20배, 5배 증가되었다. 주입 이온 선량과 에너지의 증가는 defect trap 밀도의 증가를 초래함으로, 이온 주입된 시료의 열자극 발광 세기는 이온의 선량과 에너지에 의존함을 알았다. 입사 이온의 질량이 증가함에 따라 열자극 발광 세기는 기하급수적으로 급격히 감소하였고, 이것은 열자극 발광 세기가 결함 생성률 뿐만 아니라, 이온의 주입 깊이에도 밀접한 관계가 있음을 보여주었다.