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固相萃取结合超高效液相色谱-质谱法测定畜禽肉及肉制品中肾上腺素和多巴胺的残留量

2021-10-12何亮娜马俊美范力欣李强

肉类研究 2021年9期
关键词:固相萃取

何亮娜 马俊美 范力欣 李强

摘 要:建立畜禽肉及肉制品中2 种儿茶酚胺类化合物(肾上腺素和多巴胺)的超高效液相色谱-质谱联用检测方法。样品采用10 mmol/L磷酸二氢钾溶液提取,WCX固相萃取柱净化,Waters Acquity BEH C18柱分离,采用电喷雾离子源,正离子多反应模式监测,基质匹配内标法定量。结果表明:肾上腺素和多巴胺在0.5~50 ng/mL范围内,相关系数(R2)均大于0.996;在畜肉中的检出限和定量限分别为0.39~0.40 μg/kg和1.00 μg/kg,在禽肉中的检出限和定量限分别为0.36~0.37 μg/kg和0.98 μg/kg,在肉制品中的检出限和定量限分别为0.38 μg/kg和0.96~0.97 μg/kg;加标量为1~10 μg/kg时,方法回收率为83.7%~111.2%,相对标准偏差为1.28%~5.76%。该方法具有灵敏度高、定量准确等优点,适用于畜禽肉及肉制品中残留儿茶酚胺类化合物含量的测定。

关键词:固相萃取;超高效液相色谱-质谱法;畜禽肉及肉制品;儿茶酚胺

Determination of Epinephrine and Dopamine Residues in Meat and Meat Products by Solid Phase Extraction Combined with Ultra-High Performance Liquid Chromatography-Mass Spectrometry

HE Liangna, MA Junmei, FAN Lixin, LI Qiang*

(Hebei Food Safety Key Laboratory, Hebei Food Inspection and Research Institute, Shijiazhuang 050299, China)

Abstract: An ultra-high performance liquid chromatography-mass spectrometry (UPLC-MS) method was established for the detection of the residues of two catecholamine compounds (epinephrine and dopamine) in meat and meat products. The samples were extracted with 10 mmol/L phosphate buffer solution, and the extract was purified on a WCX solid phase extraction column, and separated on a Waters Acquity BEH C18 column. The analytes were detected using an electrospray ion source in the positive ion multiple reaction monitoring (MRM) mode, and quantified by a matrix matched internal standard method. The results showed that the calibration curves for epinephrine and dopamine were linear in the concentration range of 0.5–50 ng/mL with correlation coefficient (R2) greater than 0.996. The limits of detection and limits of quantification were 0.39–0.40 and 1.00 μg/kg for livestock meat, 0.36–0.37 and 0.98 μg/kg for poultry meat, and 0.38 and 0.96–0.97 μg/kg for meat products, respectively. At spiked concentrations of 1–10 μg/kg, the recoveries of the method were between 83.7% and 111.2%, and the precision relative standard deviation (RSD) was 1.28%–5.76%. This method has the advantages of high sensitivity and accuracy, and is suitable for the determination of residual catecholamine compounds in meat and meat products.

Keywords: solid phase extraction; ultra-high performance liquid chromatography-mass spectrometry; meat and meat products; catecholamine

DOI:10.7506/rlyj1001-8123-20210422-107

中圖分类号:TS251.5                                       文献标志码:A 文章编号:1001-8123(2021)09-0027-06

引文格式:

何亮娜, 马俊美, 范力欣, 等. 固相萃取结合超高效液相色谱-质谱法测定畜禽肉及肉制品中肾上腺素和多巴胺的残留量[J]. 肉类研究, 2021, 35(9): 27-32. DOI:10.7506/rlyj1001-8123-20210422-107.    http://www.rlyj.net.cn

HE Liangna, MA Junmei, FAN Lixin, et al. Determination of epinephrine and dopamine residues in meat and meat products by solid phase extraction combined with ultra-high performance liquid chromatography-mass spectrometry[J]. Meat Research, 2021, 35(9): 27-32. DOI:10.7506/rlyj1001-8123-20210422-107.    http://www.rlyj.net.cn

肾上腺素(epinephrine,EP)和多巴胺(dopamine,DM)属于儿茶酚胺类物质,在生物体内具有增强心肌收缩力和增加血流量的作用[1-2]。EP和DM的结构式如图1所示。这2 种物质在维持机体生理平衡中起着至关重要的作用,并且其体内水平与一些病理现象息息相关[3-6]。此外,EP还具有促进动物生长的作用[7]。然而,越来越多的不法商贩为取得暴利,强行给待宰的畜禽注射儿茶酚胺类药物,以提高畜禽肉中的水分含量[8-10]。

经过该方式进行注水的畜禽肉会呈现颜色鲜红的特点,卖相较好[10]。……

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