【摘要】 目的 建立一种高效液相色谱-串联质谱法（high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS）同时检测婴幼儿辅食猪肉泥原料中38种兽药（涵盖四环素类、磺胺类、喹诺酮类、β-受体激动剂类及金刚烷胺、氯霉素、甲砜霉素等）残留的高通量分析方法。方法 样品经乙腈与乙二胺四乙酸二钠（ethylenediaminetetraacetic acid disodium salt, Na₂EDTA）-Mcllvaine缓冲溶液提取, Oasis PRiME HLB固相萃取柱净化, 40℃氮吹浓缩后,以0.2%甲酸水溶液复溶。采用Phenomenex Kinetex??2.6??m EVO C₁₈色谱柱进行分离,在安捷伦喷射流电喷雾离子源（Agilent Jet Stream electrospray ionization source, AJS ESI）,正/负离子动态切换条件下执行多反应监测,并通过空白基质匹配标准溶液法实现目标物定量分析。结果 10种目标物和28种目标物分别在10～400??g/L、10～500??g/L质量浓度区间内线性响应良好,所得相关系数（r）均不低于0.995;检出限为0.03～1.47??g/kg,定量限为0.10～4.90??g/kg。在5、10、20??g/kg 3个加标水平下进行回收率试验实验（n=6）,平均回收率为64.32%～111.66%,相对标准偏差为2.17%～10.70%,所有结果均符合GB/T 27404—2008《实验室质量控制规范食品理化检测》的相关技术要求。结论 该方法操作流程简便,兼具高灵敏度、良好的准确度与精密度,可用于婴幼儿辅食猪肉泥原料中38种兽药残留的高通量筛查与确证。更多还原

【Abstract】 Objective To establish a method for simultaneous detection of 38 kinds of veterinary drug residues（including tetracyclines, sulfonamides, quinolones, β-agonists, amantadine, chloramphenicol, thiamphenicol, etc.） in raw pork puree for infant complementary foods by high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）. Methods Samples were extracted with acetonitrile and ethylenediaminetetraacetic acid disodium salt（Na₂ EDTA）–Mcllvaine buffer, cleaned-up on an Oasis PRiME HLB cartridge, concentrated to dryness under nitrogen at 40 °C and reconstituted in 0.2% formic acid. Chromatographic separation was performed on a Phenomenex Kinetex?? 2.6 ??m EVO C₁₈ column, and the analysis was conducted using multiple reaction monitoring with dynamic polarity switching via an Agilent Jet Stream electrospray ionization source（AJS ESI）, with quantification based on a matrix-matched calibration standard approach. Results The 10 kinds of target compounds and 28 kinds of target compounds showed good linear responses in the concentration ranges of 10–400 ??g/L and 10–500 ??g/L, respectively, and the correlation coefficients（r） of the obtained calibration curves were all no less than 0.995. The limits of detection were determined to range from 0.03 to 1.47 ??g/kg, with the limits of quantitation established between 0.10 and 4.90 ??g/kg. At 3 spiked levels of 5, 10 and 20 ??g/kg（n=6）, the average recoveries ranged from 64.32% to 111.66% with relative standard deviations of 2.17%–10.70%, meeting the requirements specified in GB/T 27404—2008 Specifications for quality control in laboratories-Physical and chemical testing of food. Conclusion This method offers straightforward operation, high sensitivity, good accuracy and precision, enabling high-throughput screening and confirmation of 38 kinds of veterinary drug residues in pork puree used as raw material for infant complementary foods.更多还原