高效液相色谱-串联质谱内标法测定动物源性食品中玉米赤霉烯酮及其代谢产物
宁欣,王炼,王希希,李鹏昊
成都市疾病预防控制中心,成都 610041
Determination of zearalenone and its metabolites in animal-originated foods by HPLC-MS/MS method with internal standards
宁欣,王炼,王希希,李鹏昊
Chengdu Center for Disease Control & Prenvention, Chengdu 610041, China
摘要:建立高效液相色谱-串联质谱法(HPLC-MS/MS)测定动物源性食品中玉米赤霉烯酮及其5种代谢产物(α-玉米赤霉烯醇、β-玉米赤霉烯醇、α-玉米赤霉醇、β-玉米赤霉醇、玉米赤霉酮)残留量。在样品中加入4种同位素内标(13C18-玉米赤霉烯酮,D7-α-玉米赤霉烯醇,D7-β-玉米赤霉烯醇,D5-α-玉米赤霉醇)后,经β-葡萄糖苷酶/硫酸酯酶酶解,用叔丁基甲基醚萃取,取上清液氮吹至近干后用三氯甲烷复溶,再用氢氧化钠溶液反向萃取,以HLB固相萃取柱净化后,用HPLC-MS/MS检测。结果表明,玉米赤霉烯酮及其代谢产物在1.0~100.0 μg/L范围内线性关系良好,相关系数均大于0.996,方法的检出限为0.04~0.13 μg/kg,定量限为0.11~0.43 μg/kg。在1.0、4.0、10.0 μg/kg三种加标浓度水平下,回收率为77.7%~105.5%,测定结果的相对标准偏差为4.8%~9.8%(n=6)。该方法准确、可靠,灵敏度高,适用于动物源性食品中玉米赤霉烯酮及其代谢产物的定量分析。
Abstract:A method was established for the determination of zearalenone and its five metabolites (α-zearalanol, β-zearalanol, α-zearalenol, β-zearalenol and zearalanone) in animal-originated foods by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). By adding four isotopic internal standards (13C18-zearalenone, D7-α-zearalenol, D7-β-zearalenol, D5-α-zearalanol), the food samples were enzymolyzed by β-glucosidase/sulfatase and extracted by tert-butyl methyl ether. Being concentrated under a nitrogen stream and reconstituted in trichloromethane, the target compounds were analyzed by HPLC-MS/MS after reverse liquid-liquid extraction with sodium hydrate solution and purification with HLB solid-phase extraction cartridge. Calibration curves (1.0-100.0 μg/L) were prepared and high linearity was achieved (r>0.996). Limits of detection and quantification were 0.04-0.13 μg/kg and 0.11-0.43 μg/kg, respectively. The recoveries at the addition levels of 1.0, 4.0, 10.0 μg/kg were in the range of 77.7%-105.5%, and the relative standard deviations of determination results were 4.8%-9.8%(n=6). The method is precise, reproducible and sensitivity, which is recommended for the quantification of zearalenone and its five metabolites in animal-originated foods.
关键词:高效液相色谱-串联质谱;玉米赤霉烯酮;动物源性食品;内标法
Keywords:HPLC-MS/MS; zearalenone; animal-originated foods; internal standard method
本文引用格式:
宁欣,王炼,王希希,等.高效液相色谱-串联质谱内标法测定动物源性食品中玉米赤霉烯酮及其代谢产物[J].化学分析计量,2021,30(1):35. Ning Xin,Wang Lian,Wang Xixi,et al. Ddetermination of zearalenone and its metabolites in animal-originated foods by HPLC-MS/MS method with internal standards[J]. Chemical Analysis and Meterage,2021,30(1):35.
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