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目的建立高效毛细管电泳法(High Performance Capillary Electrophoresis,HPCE)测定棉籽油中游离棉酚含量的检测方法。方法色谱柱为未涂层石英毛细管(50cm×75μm,长度48.5cm),分离电压15kV,柱温25℃,进样量0.5pis×10s,缓冲溶液为0.10mmol/L、pH=8.00的四硼酸钠-混合磷酸溶液,检测波长235nm。结果棉酚浓度在10~100μg/mL范围内线性良好(r2=0.999 0),精密度RSD为1.2%,稳定性RSD为1.8%,检测限为1.00μg/mL,平均回收率为99.4%~100.2%,RSD为0.5%。采用该方法检测市售24批油样,其中4批样品检测到游离棉酚,含量分别为1.722、3.000、2.085、2.295μg/mL,10批样品中检测到棉酚降解产物。结论该方法准确度,精密度良好,游离棉酚的分离度较好,可以作为测定棉籽油中游离棉酚含量的方法。
Objective To establish a method for the determination of free gossypol in cottonseed oil by High Performance Capillary Electrophoresis (HPCE). Methods The column consisted of uncoated quartz capillary (50cm × 75μm, length 48.5cm), separation voltage 15kV, column temperature 25 ℃, injection volume 0.5pis × 10s, buffer solution 0.10mmol / L, pH = 8.00 Sodium - mixed phosphoric acid solution, detection wavelength 235nm. Results The linearity was good (r2 = 0.999 0) with RSD of 1.2%, RSD of stability was 1.8% and the detection limit was 1.00μg / mL. The average recovery was 99.4% ~ 100.2%, RSD 0.5%. 24 batches of oil samples were tested by this method. Free gossypol was detected in 4 batches of samples, with contents of 1.722, 3.000, 2.085 and 2.295 μg / mL, respectively. Gossypol degradation products were detected in 10 batches of samples. Conclusion The method has good accuracy and precision, and the separation of free gossypol is better, which can be used as a method to determine free gossypol content in cottonseed oil.