液相色谱串联质谱法检测鲍鱼汁中的酸性橙Ⅱ

Determination of Acid OrangeⅡ in Abalone Soup with High Performance Liquid Chromatography-Tandem Mass Spectrometry

目的建立了液相色谱/串联质谱(HPLC-MS/MS)测定鲍鱼汁中酸性橙Ⅱ的方法,并用于实际样品的分析。方法样品经甲醇+乙酸铵溶液(体积比为1+1)振荡提取后用OASISWAXSPE柱净化,以乙腈-乙酸铵缓冲溶液为流动相,在C18色谱柱(2.1mm×50mm,1.7μm)上经梯度洗脱分离后以多反应监测质谱测定(m/z326.9→170.8,326.9→155.8)。结果方法的最低定量浓度(LOQ)为0.1mg/kg,5和50mg/kg两个水平加标样的平均回收率分别为87.0%和101.0%,线性相关系数为0.999,线性范围为10～5000μg/L。对14份食品专项整治抽检样品进行分析检测,其中7份检出酸性橙Ⅱ,其含量范围为1.2～73.8mg/kg。结论该方法能够满足鲍鱼汁中酸性橙Ⅱ的测定要求。

Objective To develop an analytical method for the analysis of acid orange II in abalone soup with high performance liquid chromatography-tandem mass spectrometry （ HPLC-MS/MS）. Method Samples were extracted by methanol ＋ ammonium acetate buffer （ 1 ＋ 1, v/v） and purified on an OASIS WAX SPE column. The chromatographic column of HPLC-MS/MS was Waters Acuity BEH C18 （2. 1 mm × 50 mm, 1.7 μm）. Acid orange II was detected by monitoring the ion transition of m/z 326.9→170. 8 and 326. 9→155.8 using multiple reaction monitoring （MRM） mode. Results The limit of quantification （LOQ） was 0.1 mg/kg, and the recoveries of two spiked samples （5 mg/kg and 50 mg/kg） were 87.0% and 101% respectively. The calibration curves showed good linearity in the range of 10-5000 μg/L with correlation coefficients larger than 0. 999. The detection of acid orange II in 14 samples from restaurants showed that the concentration of acid orange II in 7 samples were 1.2-73.8 mg/g. Conclusion The method could meet the requirement for fast and accurate detection of acid orange II in abalone soup.