• 분석과학
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• 제36권2호
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• pp.89-98
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• 2023

Analytical methods for detecting atranol, chloroatranol, evernic acid, (+)-usnic acid, and atranorin in sanitary napkins and mouthwashes were developed using ultrahigh performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). UHPLC-MS/MS conditions were optimized for rapid, sensitive, and simultaneous analysis of the five allergenic compounds. The methods were validated by assessing their specificity, matrix effects, limit of detection (LOD), limit of quantification (LOQ), linearity, accuracy, and precision. Good linearity was achieved with a determination coefficient of ≥0.99. The LOD and LOQ were 2.1-9.8 and 6.4-29.6 ng/g for sanitary napkins and 0.29-0.48 and 0.87-1.45 ng/mL for mouthwashes, respectively. The accuracy and precision were within an acceptable range according to the criteria reported in the European SANTE/11813/2017 guidelines (70-120 % recovery, <20 % relative standard deviation). Therefore, these methods can be used to analyze atranol, chloroatranol, evernic acid, (+)-usnic acid, and atranorin in sanitary napkins and mouthwashes.

• 한국축산식품학회지
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• 제43권5호
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• pp.914-937
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• 2023

The objective of this study was to establish a multi-residue quantitative method for the analysis of anthelmintic and antiprotozoal drugs in various livestock products (beef, pork, and chicken) using ultra-high-performance liquid chromatography-tandem mass spectrometry. Each compound performed validation at three different levels i.e., 0.5, 1, and 2× the maximum residue limit according to the CODEX guidelines (CAC/GL 71-2009). This study was conducted according to the modified quick, easy, cheap, effective, rugged, and safe procedure. The matrix-matched calibrations gave correlation coefficients >0.98, and the obtained recoveries were in the range of 60.2%-119.9%, with coefficients of variation ≤32.0%. Furthermore, the detection and quantification limits of the method were in the ranges of 0.03-3.2 and 0.1-9.7 ㎍/kg, respectively. Moreover, a survey of residual anthelmintic and antiprotozoal drugs was also carried out in 30 samples of beef, pork, and chicken collected in Korea. Toltrazuril sulfone was detected in all three samples. Thus, our results indicated that the developed method is suitable for determining the anthelmintic and antiprotozoal drug contents in livestock products.

• 한국식품위생안전성학회지
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• 제34권5호
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• pp.413-420
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• 2019

본 연구에서는 chlorogenic acid 이성질체 9종과 arbutin을 분석하기 위하여, 전처리 과정과 UHPLC-MS/MS 동시분석 조건을 확립하였다. UHPLC-MS/MS에서 C18 column을 사용하여 15분 동안 분석할 수 있는 용매 조성을 만들고, 10가지 물질에 대한 정량, 정성 이온을 선택하여 negative 모드에서 분석하는 동시분석법을 확립하였고 과일류를 대상으로 추출, 진탕추출, 초음파 추출, 원심분리, 농축 등의 과정을 거치는 전처리법을 개발하였다. 기기분석과 전처리법에 대한 유효성은 특이성, 직선성, 정확성, 정밀성 그리고 검출한계 및 정량한계 등을 통하여 확인하였다. 회수율은 48.1-120.3%, intraday precision(RSD)는 0.4-7.9%, interday precision (RSD)는 0.0-7.2%로 확인되었다. 따라서, 본 연구에서 확립한 동시분석방법은 과일류 중 chlorogenic acid와 arbutin을 효과적으로 분석하는데 유용할 것으로 사료된다.

• ALGAE
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• 제35권2호
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• pp.177-187
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• 2020

Cyanobacteria have been widely reported to produce a variety of UV-absorbing mycosporine-like amino acids (MAAs). Herein, we reported production of the unusual MAA, mycosporine-glycine-alanine (MGA) in the cyanobacterium Sphaerospermopsis torques-reginae ITEP-024 using a newly developed UHPLC-DAD-MS/HRMS (ultra-high performance liquid chromatography-diode array detection-high resolution tandem mass spectrometry) method. MGA had previously been first identified in a red-algae, but S. torques-reginae strain ITEP-024 is the first cyanobacteria to be reported as an MGA producer. Herein, the chemical structure of MGA is fully elucidated from one-dimensional / two-dimensional nuclear magnetic resonance and HRMS data analyses. MAAs are unusually produced constitutively in S. torques-reginae ITEP-024, and this production was further enhanced following UV-irradiance. It has been proposed that MAA biosynthesis proceeds in cyanobacteria from the pentose phosphate pathway intermediate sedoheptulose 7-phosphate. Annotation of a gene cluster encoded in the genome sequence of S. torques-reginae ITEP-024 supports these gene products could catalyse the biosynthesis of MAAs. However, addition of glyphosate to cultures of S. torques-reginae ITEP-024 abolished constitutive and ultra-violet radiation induced production of MGA, shinorine and porphyra-334. This finding supports involvement of the shikimic acid pathway in the biosynthesis of MAAs by this species.