在国标GB/T 22509-2008基础上，采用液液萃取-中性氧化铝柱纯化预处理技术，优化测定芝麻油中BaP含量的HPLC-FLD方法，并从方法学角度比较其与GC-MS方法的适用性。与国标相比，本研究的HPLC-FLD法采用梯度洗脱程序。GC-MS法色谱条件为：HP-5MS毛细管柱（30 m×0.25 mm×0.25 μm），梯度升温程序，进样口和传输线温度280 ℃，脉冲不分流进样，载气流速1.2 mL/min。MS条件：EI离子源，离子源230 ℃，四级杆150 ℃，选择离子模式（SIM）定量。线性方程分别为Y=817883X+39074（R2=0.9999）和Y=1771.9X-636.6（R2=0.9997）；检测限（LOD）分别为0.037和0.062 μg/kg；加标回收率分别为82.40%~96.21%和76.21%~94.19%，对应的相对标准偏差（RSD）为3.72%~6.64%和5.18%~7.84%，检测同一芝麻油样品的BaP含量，前者略大于后者且明显高于国标（P<0.05）。从上述结果得知，两种方法均满足我国对食用油脂中BaP含量的测定要求，HPLC-FLD法在国标的基础上得到了改善，且方法的准确性：HPLC-FLD法>GC-MS法。

The high-performance liquid chromatography-fluorescence detector (HPLC-FLD) method was optimized to determine benzo[a]pyrene (BaP) in sesame oil, and its applicability was compared with that of gas chromatography-mass spectrometry (GC-MS) with regard to methodology. Based on the Chinese standard method, GB/T 22509-2008, liquid–liquid extraction and neutral alumina column purification were used for pretreatment. Compared with GB/T 22509-2008, gradient elution was used in the HPLC-FLD method. Chromatographic conditions for GC-MS were as follows: column, HP-5MS capillary column (30 m × 0.25 mm × 0.25 μm); temperature program, gradient; injection port and transfer line temperature, 280 ℃; injection mode, pulsed splitless mode; carrier gas ?ow rate, 1.2 mL/min. The MS conditions were as follows: ionization mode, electron ionization (EI); temperature of ionization source, 230°C; quadrupole temperature, 150 ℃; with single ion monitoring (SIM) mode for quantitative analysis. The linear equations, limits of detection (LODs), recovery rates, and corresponding relative standard deviation(RSDs) for HPLC-FLD and GC-MS methods were Y = 817883X + 39074 (R2 = 0.9999) and Y = 1771.9X - 636.6 (R2 = 0.9997), 0.037 and 0.062 μg/kg, 82.40%~96.21% and 76.21%~94.19%, and 3.72%~6.64% and 5.18%~7.84%, respectively. For the same sesame oil sample, the BaP content determined by HPLC-FLD was higher than that determined by GB/T 22509-2008 and was significantly higher than that determined by GC-MS (P < 0.05). The results showed that both methods met the requirements for determination of BaP content in edible oils and fats. The HPLC-FLD method was better compared with GB/T 22509-2008 and its accuracy was greater than that of GC-MS.

国家自然科学基金项目（31130042,31271884, 31271885,31471677）；“十二五”国家科技支撑计划项目（2012BAD37B01）；国家高新技术研究和开发项目（2013AA102103）