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固相萃取-超高效液相色谱串联质谱法快速测定猪尿中的赛庚啶
曲斌
0
(江苏省畜产品质量检验测试中心)
摘要:
建立了猪尿中赛庚啶的超高效液相色谱串联质谱的测定方法。猪尿样品经酸化,混合型阳离子交换固相柱萃取后,以超高效液相色谱串联质谱测定,外标法定量。本方法的测定线性范围为0.2~5.0 mg/L。在0.2、0.4、2.0 mg/L低、中、高三个浓度的回收率为80~120 %。批内、批间精密度小于20 %。本方法简便、快速、灵敏,经实际样品分析,适用于猪尿中赛庚啶的定量测定和确证。
关键词:  超高效液相色谱-串联质谱  赛庚啶  猪尿  固相萃取  残留
DOI:
投稿时间:2012-10-08修订日期:2012-10-30
基金项目:
Simple, rapid determination of cyproheptadine in pig urine by SPE-UPLC-MS/MS
(Jiangsu Quality Inspection and Testing Center for Animal Products,Nanjing,210036)
Abstract:
A simple and rapid UPLC-MS/MS method for determination of cyproheptadine in pig urine was developed and established. The sample of pig urine was acidified, and purified by SPE with mixed cation exchange column. The analyte was determined by UPLC-MS/MS with external standard for quantification. The linearity range of the method was between 0.2 and 5.0 mg/L with good coefficient. The recoveries were between 80 % and 120 %,and precision was lower than 20 % for low, middle and high concentrations. After the practice of real samples, it is shown that the method is simple, rapid, sensitive and suitable for monitoring the residue levels of cyproheptadine in pig urine.
Key words:  Cyproheptadine  UPLC-MS/MS  pig urine  SPE  residue

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