超高效液相色谱-质谱联用法检测鱼肉中23种性激素残留量

Determination of 23 kinds of sex hormones in fish using ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  QuEChERS  液相色谱-串联质谱法  雄激素  孕激素  雌激素

英文关键词:QuEChERS  liquid chromatography-tandem mass spectrometry  androgens  progesterones  estrogens

中文摘要:

      目的 采用QuEChERS快速前处理技术, 建立鱼肉中23种性激素的超高效液相色谱-串联四极杆质谱(ultra high performance liquid chromatography tandem quadrupole mass spectrometry, UPLC-MS/MS)分析方法。方法 鱼肉样品经乙腈提取后, 采用QuEChERS快速方法提取、净化, 浓缩后的目标物均采用BEH C18分离柱、多反应监测模式(multiple reaction monitoring, MRM)、外标法定量。雄激素和孕激素采用流动相0.1%甲酸水-甲醇分离, 电喷雾正离子(electronic spray ion, ESI+)扫描; 雌激素采用乙腈-水为流动相, 电喷雾负离子(ESI-)扫描。结果 23种性激素标准曲线性良好, 相关系数(r2)均大于0.99。方法的回收率范围60.93%~102.1%, 相对标准偏差(relative standard deviation, RSD, n=6)小于16.67%, 检出限(limit of detection, LOD, S/N=3)为0.0015~0.47 μg/kg。结论 该方法简单、高效、可靠性强、灵敏度高, 可用于鱼肉中的23种性激素的残留量检测。

英文摘要:

      Objective To establish a method for the determination of 23 kinds of sex hormones residues in fish meat by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)based on QuEChERS rapid preparation technology. Methods Fish meat samples were extracted with ethyl acetate, extracted and purified by QuEChERS rapid preparation technology. The concentrated extractions were separated by BEH C18 with gradient elution and identified by multiple reaction monitoring (MRM) and quantified by external standard method. Androgens and progesterone were separated by 0.1% formic acid hydro-methanol and scanned by electronic spray ion (ESI+). Estrogens were scanned by electronic spray ion (ESI?) using acetonitrile-water as mobile phase. Results The23 kinds of hormones had good linear relationships and the correlation coefficients were larger than 0.99, the average recovery rates were 60.93%-102.1%, and the relative standard deviations (RSDs, n=6) were less than 16.67%. The limits of detection (LOD, S/N=3) were 0.0015-0.47 μg/kg. Conclusion This method is simple, rapid,reliable, sensitive and efficient, which can be used for the determination of 23 kinds of sex hormones residues in fish.