Determination of Residue Amount of Tildipirosin in 4 Poultry Meat by Ultra Performance Liquid Chromatography- Tandem Mass Spectrometry
摘 要
称取均匀粉碎的禽畜肉(鸡肉、鸭肉、猪肉、牛肉)样品2.0 g于离心管中,加入70%(体积分数)乙腈溶液20 mL,涡旋混匀1 min,依次加入氯化钠2 g、无水硫酸镁5 g,以8 000 r·min-1的转速高速匀浆萃取10 min,离心后收集上清液。将上清液以每2~3 s 1滴的速率过活化好的固相萃取柱,并依次用水3 mL、甲醇3 mL洗涤,5%(体积分数)氨水甲醇溶液5 mL洗脱,收集洗脱液,于45℃吹氮至近干,用乙腈溶解残渣,并定容至1.0 mL,过0.22 μm滤膜,滤液在优化的仪器工作条件下在超高效液相色谱-串联质谱(UPLC-MS/MS)上分析。选用BEH C18色谱柱为固定相,并以不同比例的乙腈和0.1%(体积分数)三氟乙酸溶液为流动相进行梯度洗脱。质谱分析时,选择电喷雾正离子扫描模式(ESI+)和多反应监测(MRM)模式测定鸡肉、鸭肉、猪肉、牛肉等4种禽畜肉中泰地罗新的残留量。采用空白样品配制标准溶液系列,以消除基质的影响,在上述4种禽畜肉基质中,泰地罗新的质量分数均在20.0~1 200.0 μg·kg-1内与其对应的质谱响应值呈线性关系,检出限(3S/N)为3.6~6.0 μg·kg-1;在3种浓度水平上进行加标回收试验,平均回收率为92.1%~97.9%,相对标准偏差(n=6)为0.92%~6.0%。
Abstract
A portion (2.0 g) of uniformly crashed poultry meat (i.e.chicken, duck, pork, beef) was taken and added to a centrifuge tube and shaken for 1 min with 20 mL of 70% (volume fraction) acetonitrile solution. 2 g of sodium chloride, 5 g of anhydrous magnesium sulfate were added preliminarily, which was homogenized at a high speed of 8 000 r·min-1 to extract the tildipirosin (TIP). The mixture was centrifuged and all the supernatant was collected. The supernatant was passed through a solid phase extraction column at a rate of 1 dropevery 2-3 s. 3 mL of water together with 3 mL of methanol was used to rinse the column. 5 mL of 5% (volume fraction) ammonia methanol solution was used to elute the SPE. The elution was taken and evaporated to near-dryness by N2-blowing. The residue was taken up and diluted to 1.0 mL with acetonitrile. The solution was filtered through 0.22 μm filtering membrane and the filtrate was used for UPLC-MS/MS analysis under the optimized conditions. BEH C18 column was selected as stationary phase. Mixtures of (A) acetonitrile and (B) 0.1% (volume fraction) trifluoroacetate solution in various ratios was used as mobile phase in gradient elution.The ESI+ mode and MRM mode were adopted for determination of the residue amount in chicken, duck, pork and beef sample. Blanked sample was used as matrix in preparation of standard solution series to overcome the matrix. The mass fractions of TIP were all linearly related to their corresponding MS response values within 20.0-1 200.0 μg·kg-1 in the above poultry meat, with detection limits (3S/N) in the range of 3.6-6.0 μg·kg-1. Test for recovery was made by addition of standard solutions at 3 concentration levels to a matrix sample, giving values of average recovery ranged from 92.1% to 97.9%, with RSDs (n=6) of the determined values in the range of 0.92%-6.0%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202006009
所属栏目 工作简报
基金项目 广东省医学科研基金项目(B2019005,A2018438);遵义医学院博士科研启动基金项目(BS2018-02);重庆市教委大学生创新创业训练项目(201914315002)
收稿日期 2019/7/11
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备注薛莉君,讲师,硕士,主要从事药用材料的释药与缓控释应用的研究
引用该论文: XUE Lijun,LIU Bilin,YANG Yang,WANG Yuan,CHEN Min. Determination of Residue Amount of Tildipirosin in 4 Poultry Meat by Ultra Performance Liquid Chromatography- Tandem Mass Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(6): 676~681
薛莉君,刘碧林,杨洋,王园,陈敏. 超高效液相色谱-串联质谱法测定4种禽畜肉中泰地罗新残留量[J]. 理化检验-化学分册, 2020, 56(6): 676~681
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参考文献
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【9】闫超群,黎健业,张申,等.泰地罗新注射液在猪体内的药动学及生物利用度研究[J].中国农业科学, 2018,51(19):3807-3814.
【10】陈红丽,马军,张萍,等.高效液相色谱法测定泰地罗新的研究[J].畜牧与兽医, 2016,48(6):86-88.
【11】吴家鑫,刘敏,尚飞,等.亲水作用液相色谱法测定注射液中泰地罗新含量[J].现代化工, 2019,39(2):231-234.
【12】王文湘,闫超群,华成云,等.高效液相色谱-串联质谱法测定猪组织中泰地罗新残留[J].华南农业大学学报, 2018,39(6):32-38.
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