摘要
建立了豆芽中的6-苄氨基嘌呤的高效液相色谱-串联质谱法(HPLC-MS/MS)定量定性分析方法。样品经酸化甲醇2次提取后,在高效液相色谱-串联质谱仪(HPLC-MS/MS)选择反应监测(MRM)模式下测定。采用质谱定性,外标法定量。色谱柱为资生堂MGⅡ-C18(5μm 2.1 mm×150 mm)色谱柱,以0.1%甲酸水-0.1%甲酸甲醇为流动相进行梯度洗脱,流速0.3 mL/min。在优化的实验条件下,得到了较宽的线性范围和较低的定量检出限:线性范围为0.1～20.0μg/L,线性相关系数在0.999以上,定量限为:7.3μg/kg。方法的回收率和重现性较好,回收率为98.3%～106.9%之间,相对标准偏差(RSD)在1.16%～3.56%之间。该方法操作简单高效、灵敏度高、结果准确可靠,可应于豆芽中6-苄氨基嘌呤的定量及确证分析。
A method based on high performance liquid chromatography coupled with tandem mass spectrometry （ HPLC - MS/MS） was developed for determination of the residues of 6 - benzylaminopurine in bean sprout . The sample were ex- tracted twice with methanol, and then analyzed in multiple reaction monitoring （MRM） mode. and the quantification of the analytes was carried out by the external standard method. The chromatography separation was performed on a MG H - C18 （ 5μm2.1 mm ×150mm） column by gradient elution with methanol（ containing 0. 1 .% formic acid） - and water （ containing 0. 1% formic acid） as mobile phase. Sample matrix - matched calibration was used to determine the residue contents by external standard. Under the optimized detection conditions, good linearities were obtained with their correlation coefficients no less than 0. 999, the linear ranges for 6 - benzylaminopurine was 0. 1 - 20.0μg/L, The limits of quantifi- cation for 6 - benzylaminopurine was 7.3 μg,/kg. The recoveries of 6 - benzylaminopurine range from 98.3 % tol06.9 % with relative standard deviations （RSD） of 1.2 % -3.6 %. This method was simple ,effective,sensitive and waa suitable for the determination and confirmation of 6 - benzylaminopufine in bean sprout.
出处
《江西化工》
2013年第3期99-103,共5页
Jiangxi Chemical Industry
关键词
高效液相色谱-串联质谱法
6-苄氨基嘌呤
豆芽
High performance liquid chromatography coupled with mass spectrometry （HPLCMS/MS） 6 -benzylamin- opurine bean sprout
