QuEChERS-液相色谱串联质谱法测定猪肝中烯丙孕素残留量

Determination of altrenogest residues in swine liver by QuEChERS-liquid chromatography-tandem mass spectrometry

中文关键词:  烯丙孕素  猪肝  液相色谱-串联质谱法  残留

英文关键词:altrenogest  swine liver  liquid chromatography-tandem mass spectrometry  residues

中文摘要:

      目的 建立QuEChERS-液相色谱-串联质谱法(QuEChERS-liquid chromatography-tandem mass spectrometry, QuEChERS-LC-MS/MS)检测猪肝中烯丙孕素残留量的分析方法。方法 猪肝样品经β-葡萄糖醛酸酶/芳基硫酸酯酶酶解后, 用乙腈提取, 提取液用以PSA和C18为吸附剂的QuEChERS法净化, 净化液经氮吹至干用5 mmol/L甲酸铵溶液:乙腈(6:4, V:V)溶液复溶后进行LC-MS/MS分析测定。采用Acquity BEH C18 色谱柱, 以5 mmol/L甲酸溶液和乙腈为流动相进行梯度洗脱, 多反应监测模式检测, 外标法定量。结果 方法的检出限(limit of detection, LOD)和定量限(limit of quantitation, LOQ)分别为0.03 μg/kg和0.10 μg/kg。在烯丙孕素浓度为0.01~5.0 μg/L的范围内, 线性相关系数(r)为0.9997, 3个浓度水平加标回收率在73.0%~87.5%之间, 批内相对标准偏差为2.6%~4.8%, 批间相对标准偏差为4.1%~4.6%。结论 该方法简单快捷、灵敏度高、准确可靠, 适用于猪肝中痕量烯丙孕素残留量的分析。

英文摘要:

      Objective To establish a method for determination of altrenogest residues in swine liver by QuEChERS coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods The samples were digested by β-glucuronidase/arylsulfatase, and extracted with acetonitrile. Then, the extract was purified by QuEChERS with PSA and C18 sorbent. After purification, the extract was dried under nitrogen, residues were dissolved in 5 mmol/L ammonium formate solution/acetonitrile (60:40, V:V) and detected by LC-MS/MS. The samples were analyzed on an Acquity BEH C18 column with the 5 mmol/L ammonium formate solution and acetonitrile as the mobile phase under gradient elution conditions and detected by multiple reaction monitoring mode. External standard method was applied for quantitative analysis. Results The limit of detection and limit of quantitation were 0.03 μg/kg and 0.10 μg/kg, respectively. The calibration curves of altrenogest showed good linearity within the concentrations range from 0.01 to 5.0 μg/L, and the correlation coefficient (r) was 0.9997. The recoveries at 3 spiked levels were 73.0%-87.5%, the relative standard deviations of intra-assay of 2.6%-4.8% and relative standard deviations of inter-assay of 4.1%-4.6%. Conclusion This method is simple, sensitive, accurate and reliable, and suitable for practical determination of altrenogest residues in swine liver.