摘要
目的建立免疫亲和柱净化一液相色谱法测定玉米油中玉米赤霉烯酮含量的分析方法。方法样品采用乙腈-水(9:l,K:P〇提取,免疫亲和柱净化,经lnertsilODS3-C丨8柱(250 mmx4.6mm,5nm)分离,以乙腈-水-甲醇(46:46:8,为流动相进行等度洗脱,流速1.5 mL/min,柱温30°C,经荧光检测器检测,外标法定量。结果玉米赤霉烯酮在25〜2500ng/kg范围内具有良好线性,相关系数为0.99998,检出限5ng/kg,加标回收率为87.5%~107.5%,相对标准偏差为3.2%~5.8%。对调和油中米赤霉烯酮质控考核样品MyCotoxin-PT-2018-042的检测结果满意。结论该方法前处理操作简便,损失少,减少了试剂用量,灵敏度高,准确度高,适用于玉米油中玉米赤霉烯酮的检测。
Objective To establish a method for the determination of zearalenone in com oil by immunoafflnitycolumn purification-liquid chromatography. Method The sample was extracted with acetonitrile-water (9:1, V\V)and purified by immunoafflnity column, separated with Inertsil ODS3-Ci8 column (250 mm><4.6 mm, 5 fim) at theflow rate of 1.5 mL/min by isocratic elution using acetonitrile-water-methanol (46:46:8, V. V. V) as mobile phase. Thetemperature of the column oven was maintained 30 °C and the signal was detected with fluorescence detector. Thezearalenone content was quantitatively analyzed by external standard method. Results The zearalenone had goodlinear relationships in the range of 25~2500 ^ig/kg, and the correlation coefficient was 0.99998. The limit of detectionwas 5 fig/kg. The standard recovery rate was 87.5%-107.5%, with the relative standard deviations of 3.2%-5.8%.The results of the test of Mycotoxin-PT-2018-042 in the quality control sample of gibberellin in the blended oil weresatisfactory. Conclusion This method has the advantages of simple pretreatment, less loss, reduced reagent dosage,high sensitivity and high accuracy, and is suitable for the detection of zearalenone in com oil.
作者
张昆仑
陈晓明
刘玉娇
虞震
李云升
ZHANG Kun-Lun;CHEN Xiao-Ming;LIU Yu-Jiao;YU Zhen;LI Yun-Sheng(Dali Prefecture Center for Disease Control and Prevention,Dali 671000,China)
出处
《食品安全质量检测学报》
CAS
2019年第22期7750-7755,共6页
Journal of Food Safety and Quality
