Development of an Analytical Method for the Determination of Dexamethasone in Bovine Milk Using Liquid Chromatography Coupled to Tandem Mass Spectrometry

Cha, Chun-Nam; Yoo, Chang-Yeul; Lee, Sung Joong; Son, Song-Ee; Kim, Suk; Lee, Hu-Jang

doi:10.13103/jfhs.2017.32.5.418

Cited by 2 publications

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“…여러 농도의 표준용액(0.025-100 ng/mL)을 이용하여 작성한 검 량곡선의 직선성을 확인하기 위해 상관계수(coefficient of correlation, R 2 )를 구하였다. 검출한계(limit of detection, LOD)와 정량한 계(limit of quantitation, LOQ)는, 앞선 연구 [20]의 방법에 따라, 공 시료에 각 시료의 0.5 × MRL (근육, 지방, 신장: 0.05 ng/mL, 간: 0.1 ng/mL) 농도가 되도록 TML 표준용액을 가하여 전처리하여 분 석한 chromatogram에서 signal to noise ratio (S/N ratio)의 각각 3배와 10배 농도로 하였다. 회수율 측정은 근육, 간, 신장의 공시료 에 TML을 가하여 각각 0.1, 10, 100 ng/mL 농도로 만들고, 지방의 공시료에는 TML을 첨가하여 각각 0.2, 20, 200 ng/mL 농도로 만 들어, 3 반복으로 전처리하였다.…”

Section: 분석법 검증unclassified

“…또 한, 근육, 간, 신장에 대한 LOD와 LOQ는 각각 0.03과 0.1 ng/mL 였으며, 지방에 대한 LOD와 LOQ는 각각 0.06과 0.2 ng/mL였다. 와 같이, 크로마토그램 peak의 머무름 시간에 차이가 발생한 것은 분석기기의 설정 조건이 달라서 발생한 것으로 판단된다 [20]. 본 연 구에서 확립한 육계 조직 중 TML의 잔류 분석 방법은 식품공전 [19] 의 시험법과 비교해서도 분석시간이 단축되어 분석의 효율성을 증 진시켰다.…”

Section: 결과 Tml의 크로마토그램unclassified

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Establishment of withdrawal time and analysis of tiamulin residue in tissues of orally dosed broiler chickens

Kim,

Park

et al. 2023

Korean J Vet Res

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This study was conducted to investigate tiamulin (TML) residues in the edible tissues of orally dosed broiler chickens and to re-establish the withdrawal time (WT). Thirty-six healthy Ross broiler chickens were administered 0.5 (TML-1) and 2.5 kg (TML-2) per ton feed, respectively, of the drug containing TML 78 g/kg for 10 days. Twenty-four tissue samples were collected from 6 chickens in each of the TML-1 and TML-2 groups on 0, 1, 3, and 5 days after drug administration, respectively. The residual concentrations of TML were measured using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The correlation coefficient of the calibration curves was 0.9978 to 0.9998, and the limits of detection and the limits of quantification (LOQ) were in the range of 0.03 to 0.06, and 0.1 to 0.2 µg/kg, respectively. Recoveries ranged between 89.0% to 116.7%, and the coefficients of variation were less than 13.9%. After the drug administration, TML in the TML-1 and TML-2 groups was detected above the LOQ in 1 and 6 samples of liver, respectively, at day 0, and in 1 liver sample from both groups on day one. At 3 days after administration, TML was detected below the LOQ in all samples of TML-1 and TML-2. The calculated WT of TML in both TML-1 and TML-2 using the WT calculation program WT 1.4 was 0 days. In conclusion, the developed analytical method is suitable for detection, and the calculated WT of TML in poultry edible tissues is shorter than the current recommended WT of 7 days for TML in broiler chickens.

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Section: 분석법 검증unclassified

Section: 결과 Tml의 크로마토그램unclassified

Establishment of withdrawal time and analysis of tiamulin residue in tissues of orally dosed broiler chickens

Kim,

Park

et al. 2023

Korean J Vet Res

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Establishment of withdrawal time and analysis of dexamethasone residue in milk of intramuscularly dosed cows

Park¹,

Jin²,

Kim³

et al. 2022

Korean J Vet Res

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This study investigated dexamethasone (DXM) residues in the milk from intramuscularly dosed dairy cows and established the withdrawal time (WT) of DXM in milk. Eighteen healthy Holstein cows were injected with 20 (DXM-1) or 40 mL (DXM-2) of a drug containing 1 mg/mL of DXM. After administering DXM, milk samples were collected from all cows at 12-hour intervals for five days. The DXM residue concentrations in milk were determined by liquid chromatography-mass spectrometry/mass spectrometry. The correlation coefficient of the calibration curve was 0.9966, and the limits of detection and quantification (LOQ) were 0.03 and 0.1 μg/kg, respectively. The recoveries were 97.0% to 104.0%, and the coefficient of variations was less than 7.22%. After treatment, DXM in DXM-1 was detected above the LOQ in two milk samples at 36 hours and below the LOQ in all milk samples of DXM-2 at 48 hours. Using the WT calculation program WT 1.4, the withdrawal periods of DXM-1 and DXM-2 in milk were established to be two days. In conclusion, the developed analytical method is sensitive and reliable for detecting DXM in milk. The estimated WT of DXM in bovine milk is shorter than the current milk WT recommendation of three days for DXM in lactating dairy cows.

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Development of an Analytical Method for the Determination of Dexamethasone in Bovine Milk Using Liquid Chromatography Coupled to Tandem Mass Spectrometry

Cited by 2 publications

References 0 publications

Establishment of withdrawal time and analysis of tiamulin residue in tissues of orally dosed broiler chickens

Establishment of withdrawal time and analysis of tiamulin residue in tissues of orally dosed broiler chickens

Establishment of withdrawal time and analysis of dexamethasone residue in milk of intramuscularly dosed cows

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