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,2.5μm),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0.01~0.10mg/L范围内线性良好(r2>0.999),本方法的定量限为10μg/kg。游离棉酚在10~100μg/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。
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,2.5μm)with t he 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 10μg/kg.The recoveries rate of free gossypol in the range of 10-100μg/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.
作者
贾丽华
王建山
王一欣
林芳
赵俊楠
李涛
JIA Li-Hua;WANG Jian-Shan;WANG Yi-Xin;LIN Fang;ZHAO Jun-Nan;LI Tao(Shaanxi Institute for Food and Drug Control,Xi'an 710065,China)
出处
《食品安全质量检测学报》
CAS
2020年第7期2185-2189,共5页
Journal of Food Safety and Quality
基金
2019年陕西省创新能力支撑计划项目(2019PT-22)。
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
free gossypol
ultra performance liquid chromatography-tandem mass spectrometry
animal-origin foods
