超高效液相色谱-串联质谱法测定猪肉和猪肝中烯丙孕素残留

Determination of altrenogest in swine muscle and liver by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  烯丙孕素  可食性组织中  残留检测

英文关键词:ultra performance liquid chromatography-mass spectrometry  altrenogest  edible tissue  residue detection

中文摘要:

      目的 建立猪肉和猪肝中烯丙孕素残留测定的超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)。方法 肌肉和肝脏样品, 经β-葡萄糖醛酸酶/芳基硫酸酯酶酶解、乙腈提取、乙腈饱和正己烷溶液除脂; 经乙酸乙酯溶解后, 用10%碳酸钠溶液净化, UPLC-MS/MS测定, 外标法定量。结果 烯丙孕素在猪肉和猪肝中的检测限为0.5 μg/kg, 定量限为1.0 μg/kg; 在1.0、2.0和5.0 μg/kg浓度添加的回收率为68.8%~87.6%、日内相对标准偏差(relative standard deviation, RSD)为1.8%~8.9%, 日间RSD为1.8%~6.9%。结论 该方法操作简便、准确、重现性好, 适用于猪肌肉、肝脏中烯丙孕素残留物含量测定。

英文摘要:

      Objective To establish a method for determination of altrenogest residues in swine muscle and liver by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The liver and muscle samples were hydrolyzed by β-glucosidase/arysulfatase and extracted by acetonitrile, then the extracting solution were degreased with n-hexane. After being dissolved with ethyl acetate, the supernatant was purified by 10% sodium carbonate solution. Finally, altrenogest was analyzed by UPLC-MS/MS, and the external method was used. Results Altrenogest had good linearities in the range of 1-200 ng/mL, and the correlation coefficients (r2) were more than 0.99. The limit of quantification was 1.0 μg/kg, and the limit of detection was 0.5 μg/kg. At 3 spiked levels of 1.0, 2.0 and 5.0 μg/kg, the average recoveries were 68.8%-87.6% for altrenogest, with intra-day relative standard deviations (RSDs) of 1.8%-8.9% and inter-day RSDs of 1.8%-6.9%. Conclusion This method is simple, effective and sensitive, which is suitable for determination of altrenogest in swine muscle and liver.