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Determination Method for Ractopamine in Swine and Cattle Tissues Using LC/MS

机译:LC / MS测定猪和牛组织中莱克多巴胺的方法

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Simple and reliable methods using LC/MS have been developed for the determination of the β-agonist ractopamine in swine and cattle tissues. Ractopamine was extracted with ethyl acetate from muscle and liver, and the ethyl acetate layer was evaporated to dryness. The residue was purified by partition with acetonitrile-hexane. In the case of fat, ractopamine was extracted and purified by partition with acetonitrile-hexane. The resulting acetonitrile solutions were evaporated to dryness. The residue was dissolved in methanol, and subjected to LC/MS. The LC separation was performed on a Wakosil-Ⅱ 3C18HG column (150 × 3 mm i.d.) in isocratic mode with 0.05% trifluoroacetic acid-acetonitrile (80 : 20) as a mobile phase at a flow rate of 0.4 mL/min. The MS detection was performed in the selected ion recording (SIR) mode, with detection of the M + H~+ ion of ractopamine (m/z 302) produced by electrospray ionization (ESI). The mean recoveries of the drug from swine muscle (0.01 μg/g fortified), fat (0.01μg/g fortified) and liver (0.04 μg/g fortified) were 99.7%, 99.5% and 100.8%, and those from cattle samples were 108.3%, 97.0% and 109.4%, respectively. The relative standard deviations (RSDs) ranged from 0.1% to 9.5%. The limit of quantification (LOQ) of the drug was 1 ng/g.
机译:已经开发出使用LC / MS的简单可靠的方法来测定猪和牛组织中的β-激动剂莱克多巴胺。用乙酸乙酯从肌肉和肝脏中提取莱克多巴胺,并将乙酸乙酯层蒸发至干。残余物通过用乙腈/正己烷分配而纯化。在脂肪的情况下,提取莱克多巴胺并通过与乙腈/正己烷分配进行纯化。将所得乙腈溶液蒸发至干。将残余物溶解在甲醇中,并进行LC / MS。 LC分离在Wakosil-Ⅱ3C18HG色谱柱(150×3 mm i.d.)上,以等度模式,以0.05%三氟乙酸-乙腈(80:20)为流动相,流速为0.4 mL / min。 MS检测在选定的离子记录(SIR)模式下进行,同时检测通过电喷雾电离(ESI)产生的莱克多巴胺(m / z 302)的M + H +离子。从猪肌肉(强化的0.01μg/ g),脂肪(强化的0.01μg/ g)和肝脏(强化的0.04μg/ g)的平均回收率分别为99.7%,99.5%和100.8%,而从牛样品得到的回收率分别为分别为108.3%,97.0%和109.4%。相对标准偏差(RSD)为0.1%至9.5%。该药物的定量限(LOQ)为1 ng / g。

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