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目的建立猪肉中6种玉米赤霉醇类物质(α-玉米赤霉醇、β-玉米赤霉醇、α-玉米赤霉烯醇、β-玉米赤霉烯醇、玉米赤霉酮和玉米赤霉烯酮)的超高压液相色谱-串联质谱(UPLC-MS/MS)检测方法。方法样品经β-葡萄糖苷酶/硫酸酯酶酶解,无水乙醚萃取,再经氢氧化钠溶液液-液分配,最后通过HLB固相萃取柱富集净化,UPLC-MS/MS检测,基质匹配外标标准曲线法定量。结果 6种玉米赤霉醇类物质的线性范围为1.0~250μg/L,相关系数r>0.990。当取样量为5.0g时,6种玉米赤霉醇类物质检出限为0.4μg/kg。3个不同水平(添加1.0、5.0、20μg/kg)的加标平均回收率为66.0%~79.5%,相对标准偏差不大于10%。结论所建立的方法具有较好的回收率和精密度,准确度和灵敏度高,符合猪肉中玉米赤霉醇类物质痕量的检测要求,为大通量样品的食品安全检测提供更灵敏、高效的技术支持。
Objective To establish a method for the determination of 6 kinds of zearalenol in pork (α- zearalenol, β-zearalenol, α-zearalenol, β-zearalenol, (HPLC-MS / MS) method was developed. Methods The samples were digested by β-glucosidase / sulfatase, extracted with anhydrous ether, and then liquid-liquid partitioned by sodium hydroxide solution. Finally, the samples were purified by HLB solid phase extraction column, UPLC-MS / MS, Matching external standard curve method of quantitative. Results The linear ranges of the 6 kinds of zearalenol were 1.0-250 μg / L with the correlation coefficient r> 0.990. When the sample volume was 5.0g, the detection limit of 6 kinds of zearalenol was 0.4μg / kg. The spiked average recoveries of three different levels (1.0, 5.0 and 20 μg / kg) were 66.0% -79.5% with relative standard deviations less than 10%. Conclusion The established method has good recovery and precision, high accuracy and sensitivity, meets the detection requirements of trace amounts of zearalenol in pork, and provides more sensitive and efficient food safety testing for large sample throughput Technical support.