• 한국축산식품학회지
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• 제41권5호
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• pp.816-825
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• 2021

This study aims to validate a fast method of simultaneous analysis of 365 LCamenable and 142 GC-amenable pesticides in hen eggs by liquid chromatography-tandem mass spectrometry (LC-MS/MS) and gas chromatography-tandem mass spectrometry (GC-MS/MS), respectively, operating in multiple reaction monitoring (MRM) acquisition modes. The sample preparation was based on quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction. Key method performance parameters investigated were specificity, linearity, limit of quantification (LOQ), accuracy, precision and measurement uncertainty. The method was validated at two spiking levels (10 and 50 ㎍/kg), and good recoveries (70%-120%) and relative standard deviations (RSDs) (≤20) were achieved for 92.9% of LC-amenable and 86.6% of GC-amenable pesticide residues. The LOQs were ≤10 ㎍/kg for 94.2% of LC-amenable and 92.3% of GC-amenable pesticides. The validated method was further applied to 100 egg samples from caged hens, and none of the pesticides was quantified.

• Mass Spectrometry Letters
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• 제3권2호
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• pp.29-38
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• 2012

A new approach of volatile compounds analysis is proposed using a linear ion trap Orbitrap mass spectrometer coupled with gas chromatography through an atmospheric pressure photoionization interface. In the proposed GC-HRMS/MS approach, direct chemical composition analysis is made for the precursor ions in high resolution MS spectra and the structural identifications were made through the database search of high quality MS/MS spectra. Successful analysis of a complex perfume sample was demonstrated and compared with GC-EI-Q and GC-EI-TOF. The current approach is complementary to conventional GC-EI-MS analysis and can identify low abundance co-eluting compounds. Toluene co-sprayed as a dopant through API probe significantly enhanced ionization of certain compounds and reduced oxidation during the ionization.

• Mass Spectrometry Letters
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• 제14권3호
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• pp.104-109
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• 2023

Anabolic-androgenic steroids (AAS) are used illegally to enhance muscle development and increase strength and power. In this study, a reliable, and sensitive quantitative method was developed and validated using heptafluorobutyric acid anhydride (HFPA) derivatives for the simultaneous detection of prohibited AAS (testosterone [TS], boldenone [BD], 5α-estrane-3β,17α-diol [EAD]) using gas chromatography-tandem mass spectrometry (GC-MS/MS). For processing the samples, solid phase extraction, methanolic hydrolysis, and liquid-liquid extraction were used. For detection using mass spectrometry, the multiple reaction monitoring (MRM) mode was used with the electron ionization (EI) positive mode. The method was evaluated for selectivity, linearity, lower limit of quantification, intra- and inter-day precision, accuracy, and stability. The results showed that the method was accurate and reproducible for the quantitation of the three steroids. The developed method was finally applied to the analysis of a suspect gelding urine sample received from the Asian Quality Assurance Program (AQAP).

• Bulletin of the Korean Chemical Society
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• 제10권2호
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• pp.196-200
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• 1989

Some s-triazine herbicides, namely simazine, atrazine, and propazine present as trace components in a complex mixture were analyzed by GC/MS and GC/MS/MS methods. Even though monitoring the molecular ions was the best in terms of sensitivity, adequate analysis could not be done when interfering species were present. When doubly charged ions which appeared at characteristic m/z values were monitored, chromatograms were rather free from interference. More importantly, selected reaction monitoring was found to provide a selective means of detection with general applicability.

• Bulletin of the Korean Chemical Society
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• 제26권4호
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• pp.575-578
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• 2005

Electrospray ionization mass spectrometry (ESI MS) was used, along with gas chromatography-mass spectrometry (GC-MS), to monitor Paal-Knorr synthesis of 2,5-dimethyl-1-phenylpyrrole by condensation of aniline with 2,5-hexanedione. In addition to 2,5-dimethyl-1-phenylpyrrole observed as a single spot by TLC, unexpected dimer size compounds were observed by GC-MS. Dimers and trimers were observed by ESI MS. ESI tandem mass spectrometry was used to select plausible structures for the dimer. ESI MS with or without liquid chromatographic separation is useful for observing oligomeric byproducts with low volatility produced in organic reactions.

• 대한환경공학회지
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• 제36권6호
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• pp.387-395
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• 2014

본 연구에서는 SBSE 전처리 장치와 GC-MS/MS를 이용하여 합성 향물질 11종을 동시 분석할 수 있는 분석법을 개발하기 위해 흡착 bar의 교반시간, 교반속도, 시료수의 pH, 시료수 용량, 염석제 투입량 및 메탄올 주입량 변화 등 SBSE (stir bar sorptive extraction) 전처리 조건과 GC-MS/MS (gas chromatography/tandem mass spectrometry)의 기기조건을 다양하게 변화시켜 SBSE-GC-MS/MS를 이용한 분석법을 개발하였다. 11종의 합성 향물질들에 대한 검출한계(LOD)는 2.1~4.1 ng/L였으며, 정량한계(LOQ)는 6.6~12.9 ng/L였다. 수돗물, 낙동강 원수, 하수처리장 최종방류수 및 해수를 이용하여 시료수의 matrix 영향을 살펴본 결과, 11종의 합성 향물질들의 회수율 및 RSD의 경우 각각 88%~119% 및 0.8%~7.5%로 양호한 결과를 나타내어 시료수의 matrix 영향을 받지 않는 것으로 나타났다. 본 연구에서 개발된 SBSE-GC-MS/MS 분석법은 40 mL 정도의 적은 시료수량으로도 고감도 분석이 가능하며, 용매류를 사용하지 않기 때문에 분석자의 건강 및 환경친화적인 분석법이라는 장점뿐만 아니라 간편하고, 빠르며 자동화된 방법이라는 장점을 가진다.

• Mass Spectrometry Letters
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• 제12권2호
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• pp.31-40
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• 2021

Probable human carcinogenic compounds nitrosamines, have been detected as by-product impurities in sartan pharmaceuticals in recent years which has drawn worries for medication safety. To provide a sensitive and effective method for the quality control of sartan pharmaceuticals, this study established a feasible gas chromatography-tandem mass spectrometry (GC-MS/MS) method for simultaneous determination of 13 nitrosamines. The target analytes were separated on a DB-WAX Ultra Inert column (30 m × 0.25 mm; i.d., 0.25 ㎛) and were then subjected to electron impact ionization in multiple reaction monitoring mode. The established method was validated and further employed to analyze authentic samples. Limits of detection (LODs) and limits of quantification (LOQs) of the 13 nitrosamines were 15-250 ng/g and 50-250 ng/g, respectively, which also exhibited intra-day and inter-day accuracies of 91.4-104.8%, thereby satisfying validation criteria. Five nitrosamines, viz., N-nitrosodiethylamine, N-nitrosodimethylamine, N-nitrosodiphenylamine, N-nitrosomorpholine, and N-nitrosopiperidine were detected at concentrations above their LODs in 68 positive samples out of 594 authentic samples from seven sartans.

• 분석과학
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• 제36권5호
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• pp.205-215
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• 2023

In the present study, an analytical method was proposed for detecting trifluralin in aquatic products at trace concentrations. The method employed QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) and gas chromatography coupled with tandem mass spectrometry (GC-MS/MS) as the sample preparation and measurement, respectively. The effect of the aqueous phase volume used in the QuEChERS was demonstrated, and the ratio of 10:10 (mL) between water and acetonitrile phase was used for 5 g of sample. Besides, dSPE using C18 and primary-secondary amine (PSA) was applied to remove the potential interferences from the food matrices, indicating no remarkable analyte loss. The linear range was built up from 0.50 ㎍ L^-1 to 3.0 ㎍ L^-1 (R² = 0.9993). Other criteria, i.e., repeatability (RSD_r = 0.86-1.96 %), reproducibility (RSD_R = 1.09-2.01 %), and recovery (over 90 %), were in accordance with Appendix F of AOAC (2016) for method performance. Although no trifluralin was detected for the commercial samples (fish, shrimp, and breaded shrimp), the spiked samples performed favorable recoveries and precision.

• 한국환경과학회지
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• 제23권6호
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• pp.1037-1047
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• 2014

A highly sensitive analytical method based on stir bar sorptive extraction (SBSE) technique and gas chromatography/tandem mass spectrometry (GC/MS-MS) has been developed, allowing the simultaneous multi-analyte determination of seven UV filters in water samples. The stir bar coated with polydimethylsiloxane (PDMS) was added to 40 mL of water sample at pH 3 and stirred at 1,100 rpm for 120 min. Other SBSE parameters (salt effect and presence of organic solvent) were optimised. The method shows good linearity (coefficients > 0.990) and reproducibility (RSD < 12.9%). The extraction efficiencies were above 84% for all the compounds. The limits of detections (LOD) and limits of quantification (LOQ) were 2.1~8.6 ng/L and 6.8~27.5 ng/L, respectively. The developed method offers the ability to detect 8 UV filters at ultra-low concentration levels with only 40 mL of sample volume. Matrix effects in tap water, river water, wastewater treatment plant (WWTP) final effluent water and seawater were investigated and it was shown that the method is suitable for the analysis of trace level of 7 UV filters except of benzophenone (BP). The method developed in the present study has the advantage of being rapid, simple, high-sensitive and both user and environmentally friendly.

• 한국식품위생안전성학회지
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• 제33권2호
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• pp.110-117
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• 2018

본 연구는 국내 생산 및 수입 양식 수산물에 대해 잔류할 수 있는 향정신성 의약품인 디아제팜 대한 안전관리강화기반을 위해 마련되었다. 중국인민공화국 국가 표준시험법(GB 29697-2013)을 기반으로 전처리 방법을 개선하여 GC-MS/MS 시험법을 확립하였으며, LC-MS/MS 방법과의 기기간 검증을 통해 확립된 시험법의 선택성, 정량한계 및 회수율에 대한 검증을 통해 디아제팜 시험법으로서의 유효성을 확인하였다. LC-MS/MS의 경우 아세토니트릴로 추출 후 PSA를 이용해 정제하였고, GC-MS/MS의 경우 아세토니트릴로 추출후 $C_{18}$카트리지를 이용해 정제하였다. 디아제팜은 표준용액을 정량한계를 포함한 농도에 따라 검량선을 작성한 결과 두 기기 모두 $r^2$> 0.99 이상의 직선성을 확인하였다. 본 실험에서의 검출한계와 정량한계는 LC-MS/MS 및 GC-MS/MS 모두 0.0004 mg/kg, 0.001 mg/kg 수준이었으며, 평균 회수율은 각각 99.8~106%, 109~124%이었다. 또한, 분석오차는 모두 15% 이하로 정확성 및 재현성이 우수하였으며, CODEX 가이드라인 규정에 만족하는 수준이었다. 따라서 개발된 시험법은 안전한 수산물의 국내 유통과 잔류실태조사를 위해 활용될 것으로 기대한다.