Hu Li, Lei Shaorong, Guo Ling'an
Center of Analysis and Testing, Sichuan Academy of Agricultural Sciences, Chengdu 610066, China.
Se Pu. 2012 Aug;30(8):832-5. doi: 10.3724/sp.j.1123.2012.03045.
An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/ MS) method was developed for the determination of citrus red 2 (CR2) in navel orange. The sample was extracted with acetonitrile, cleaned-up by an NH2 solid phase extraction cartridge. Then, the analyte was separated on a Waters Acquity UPLC BEH C18 column (50 mm x 2.1 mm, 1.7 microm) in gradient elution with the mobile phases of water and acetonitrile. The separated compounds were detected with a Waters Xevo TQ MS tandem quadrupole mass spectrometer operated in multiple reaction monitoring (MRM) mode via positive electrospray ionization (ESI+). The linearity of the method was good (r2 = 0.996 5) over the concentration range from 0.1 to 100 microg/L for CR2. The limit of detection (LOD) was 0.05 microg/kg, and the limit of quantification (LOQ) was 0.1 microg/kg. The average recoveries of CR2 at the three levels of 1.0, 10.0 and 100.0 microg/kg were between 84.2% and 94.0% with the relative standard deviations (RSDs) between 2.86% and 10.15%. Finally, a total of 18 navel orange samples randomly collected from different markets were detected by the proposed method, and two samples contained CR2. The sensitivity, accuracy, and precision of this method can meet the requirements of the CR2 analysis.
建立了一种超高效液相色谱-串联质谱(UPLC-MS/MS)法测定脐橙中柑橘红2(CR2)的含量。样品用乙腈提取,经NH2固相萃取小柱净化。然后,在Waters Acquity UPLC BEH C18柱(50 mm×2.1 mm,1.7μm)上,以水和乙腈为流动相进行梯度洗脱分离分析物。分离后的化合物采用Waters Xevo TQ MS串联四极杆质谱仪,通过正电喷雾电离(ESI+)在多反应监测(MRM)模式下进行检测。该方法在CR2浓度范围为0.1~100μg/L时线性良好(r2 = 0.996 5)。检测限(LOD)为0.05μg/kg,定量限(LOQ)为0.1μg/kg。CR2在1.0、10.0和100.0μg/kg三个加标水平下的平均回收率在84.2%~94.0%之间,相对标准偏差(RSDs)在2.86%~10.15%之间。最后,用该方法对随机从不同市场采集的18个脐橙样品进行检测,有两个样品含有CR2。该方法的灵敏度、准确度和精密度能够满足CR2分析的要求。