超高效液相色谱-串联质谱法测定动物源性食品中游离棉酚

Determination of free gossypol in animal-origin food by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  游离棉酚  超高效液相色谱-串联质谱法  动物源性食品

英文关键词:free gossypol  ultra performance liquid chromatography-tandem mass spectrometry  animal-origin foods

中文摘要:

      目的 建立超高效液相色谱-串联质谱测定动物源性食品中游离棉酚的方法。方法 样品经高速匀浆后用乙腈提取后, 经乙腈饱和正己烷去脂, 用XSelect HSS T3柱(2.1 mm×100 mm, 2.5 μm), 以含0.1%(V/V)甲酸溶液和乙腈作为流动相进行梯度洗脱, 采用电喷雾电离(electrospray ionization, ESI)和多离子检测模式(multiple reaction monitoring, MRM)进行检测, 基质匹配外标法定量。结果 在0.01~0.10 mg/L范围内线性良好（r2＞0.999）, 本方法的定量限为10 μg/kg。游离棉酚在10~100 μg/kg添加浓度范围内, 回收率为83.3%~89.2%, 相对标准偏差为3.9%~7.2%。结论 该方法准确性强, 重复性好, 灵敏度高, 可用于动物源性食品中游离棉酚的测定和确证。

英文摘要:

      Objective To establish a method for the determination of free gossypol in animal-origin food by ultra performance liquid chromatography-tandemmass spectrometry. Methods Samples were extracted with acetonitrile after high-speed homogenizationand the supernatant was degreased with n-hexane. The liquid was performed on XSelect HSS T3 (2.1 mm×100 mm, 2.5 μm)with the gradient elution of 0.1% (V/V) formic acid aqueous solution (A) and acetonitrile solution (B). The sample was detectedby electrospray ionization (ESI) with multiple reactions monitoring (MRM), and quantified by matrix matched with external standard method. Results Within the range of 0.01~0.10 mg/L, the linearity was good (r2＞0.999).The quantitative limit of the method was 10 μg/kg. The recoveries rate of free gossypol in the range of 10-100 μg/kg was 83.3%–89.2% and relative standard deviation(RSD) was 3.9%–7.2%. Conclusion This method is simple, fastandreliable, which can be used for rapid screening and confirmation of free gossypol in animal-origin foods.