液相色谱-串联质谱法测定食用植物油中的棉酚

Determination of gossypol in edible vegetable oil with high performance liquid chromatography-tandem mass spectrometry

建立了食用植物油中棉酚的液相色谱-串联质谱（ LC-MS / MS）分析方法。待测物经无水乙醇涡旋振荡提取， C18色谱柱分离，以乙腈和0.1％（v / v）甲酸水溶液为流动相进行梯度洗脱，LC-MS / MS 测定，外标法定量。方法的测定低限（S / N﹥10）为1 mg / kg；在添加浓度为1、2和200 mg / kg 水平下，棉酚的加标回收率为87.4％~100％，相对标准偏差为3.9％~12.2％。结果表明，本方法灵敏度高，测定结果准确，回收率稳定，可用于食用植物油中棉酚残留的确证检测。

A liquid chromatography-tandem mass spectrometry （ LC-MS / MS ） method was developed for the determination of gossypol in edible vegetable oil. The sample was extracted with ethyl alcohol by vortex-excited oscillation. The extract was cleaned up by 0. 22 μm filter membrane and centrifuged for 5 min at 4 000 r / min after standing in a fridge at 4 ℃ for 30 min. The compound was separated on a C18 column（100 mm×2. 1 mm,3. 5 μm）with acetonitrile and 1% （ v / v）formic acid aqueous solution as mobile phase. The detection of gossypol was carried out by LC-MS / MS with positive electrospray ionization under multiple reaction monito-ring（ MRM）mode using external standard method. The limits of quantification（ S / N ﹥ 10）of gossypol in edible vegetable oil was 1 mg / kg. The recoveries were from 87. 4% to 100% at the spiked levels of 1,2,200 mg / kg of gossypol in edible vegetable oil with the relative standard deviations（RSDs）between 3. 9% and 12. 2% . The method,with high sensitivity,good preci-sion and high recovery,was suitable for the confirmation and quantification of gossypol residue in edible vegetable oil.