• 분석과학
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• 제32권2호
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• pp.35-47
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• 2019

In this study, high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was employed to detect 26 antidiabetic compounds in adulterated dietary supplements using a simple, selective method. The work presented herein may help prevent incidents related to food adulteration and restrict the illegal food market. The best separation was obtained on a Shiseido Capcell Pak(R) C18 MG-II ($2.0mm{\times}100mm$, $3{\mu}m$), which improved the peak shape and MS detection sensitivity of the target compounds. A gradient elution system composed of 0.1 % (v/v) formic acid in distilled water and methanol at a flow rate of 0.3 mL/min for 18 min was utilized. A triple quadrupole mass spectrometer with an electrospray ionization source operated in the positive or negative mode was employed as the detector. The developed method was validated as follows: specificity was confirmed in the multiple reaction monitoring mode using the precursor and product ion pairs. For solid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL, and for liquid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL. Satisfactory linearity was obtained from calibration curves, with $R^2$ > 0.99. Both intra and inter-day precision were less than 13.19 %. Accuracies ranged from 80.69 to 118.81 % (intra/inter-day), with a stability of less than 14.88 %. Mean recovery was found to be 80.6-119.0 % and less than 13.4 % RSD. Using the validated method, glibenclamide and pioglitazone were simultaneously determined in one capsule at concentrations of 1.52 and 0.53 mg (per capsule), respectively.

• 분석과학
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• 제30권5호
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• pp.262-269
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• 2017

금강수계 하천 및 호소 퇴적물에 대하여 천연 방사성핵종 농도를 조사하였다. 조사의 대상이 되는 지점은 하천 17 개 지점, 호소 6 개 지점으로 총 23 개 지점이며, 하천은 2015년 9월부터 11월, 호소는 2015년 3월부터 4월까지 시료를 채취하였다. 분석 대상 핵종은 $^{226}Ra$ 계열, $^{232}Th$ 계열과 $^{40}K$ 핵종이며, 고순도 게르마늄 검출기(HPGe)를 이용하여 대상 핵종 또는 그 자핵종이 방출하는 감마선을 계측하였다. 분석 결과 하천 퇴적물 중 $^{226}Ra$계열, $^{232}Th$ 계열과 $^{40}K$의 방사성핵종 농도는 각각 $15.6{\pm}0.6$, $33.8{\pm}1.2$, $789.8{\pm}26.0Bq/kg$ 으로 나타났으며, 호소 퇴적물의 농도는 각각 $17.0{\pm}0.5$, $37.8{\pm}1.1$, $269.4{\pm}9.6Bq/kg$으로 나타났다. $^{232}Th$ 계열 방사성핵종의 농도는 퇴적물 입도와 연관성을 보였으며, 핵종의 이동 특성에 따라 $^{226}Ra$ 계열보다 높게 나타났다. $^{40}K$의 농도는 퇴적물 중 유기물 함량과 관련을 보였으며, 하천에 비하여 호소에서 낮은 농도로 조사되었다.