Analysis of tetracyclines in chicken tissues and dung using LC–MS coupled with ultrasound-assisted enzymatic hydrolysis
Analysis of tetracyclines in chicken tissues and dung using LC–MS coupled with ultrasound-assisted enzymatic hydrolysis
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DOI：
10.1016/j.foodcont.2014.05.015
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发表时间：
2014-12
期刊：
影响因子：
6
通讯作者：
Qian Zhou;Yingying Zhang;Nan Wang;Lihua Zhu;Heqing Tang
中科院分区：
文献类型：
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作者：
Qian Zhou;Yingying Zhang;Nan Wang;Lihua Zhu;Heqing Tang
准确检测与养鸡相关的复杂基质中的四环素类抗生素(TCS)对食品控制具有重要意义。实验证明，传统的酸去蛋白方法会导致TCS的高损失，因为TCS强烈地结合在蛋白质聚集体上。为了消除这种影响，开发了一种超声波辅助的酶解法来破坏蛋白质的三维结构并释放结合的TCS。这不仅显著提高了天冬氨酸的回收率，而且使前处理时间从960分钟缩短到6分钟。将这种新的脱蛋白方法与固相萃取净化相结合，获得了适合于天花粉蛋白LC-MS/MS分析的样品前处理方法，建立的天花粉蛋白的LC-MS/MS分析方法线性范围为20~1000gμg/L−1，检出限为1.0 5~3.50gμg/L−1。新方法在鸡肉相关样品中的加标回收率高达89.1%~102.4%，远高于酸脱蛋白法的回收率(23.5%~36.2%)。用该方法对5个实际粪便样品进行分析，土霉素和金霉素的残留量分别为0.94.2 mg/kg−1和1.3-4.0mgkg-1。
The accurate measurement of tetracycline antibiotics (TCs) in complex matrices related to chicken raising is important for food control. It was experimentally demonstrated that conventional acid deproteination methods led to high losses of TCs because TCs were strongly bounded to protein aggregates. To eliminate this effect, an ultrasound-assisted enzymatic hydrolysis method was developed to break the three-dimensional structures of proteins and release the bound TCs. This not only significantly improved the recovery of TCs but also shortened the pretreatment time from 960 to 6 min. By combining this new deproteination method and a solid phase extraction clean-up, a suitable sample preparation was achieved for the analysis of TCs with LC–MS/MS. The established LC–MS/MS analysis of TCs provided good linear ranges in the order of 20–1000 μg L−1with the limits of detection ranging from 1.05 to 3.50 μg L−1for the tested TCs. The new method yielded recoveries of TCs in spiked chicken-related samples as high as 89.1%–102.4%, being much higher than those (23.5%–36.2%) obtained using the acid deproteination process. When this method was used to analyze five practical samples of manures, it gave residual concentrations of 0.9–4.2 and 1.3–4.0 mg kg−1for oxytetracycline and chlortetracycline, respectively.