HPLC-ELSD法测定破壁灵芝孢子粉中8个油脂类成分的含量

Determination of eight lipin components in Ganoderma lucidum spore powder by HPLC-ELSD

目的:采用HPLC-ELSD建立灵芝孢子粉中8种油脂类成分的含量测定方法。方法:采用ACCHROM Unitary-C_(18)色谱柱(250 mm×4.6 mm,5μm),流动相为乙腈-异丙醇(51∶49),流速1.0mL·min^(-1),柱温30℃,检测器为蒸发光散射检测器(漂移管温度105℃,载气流速2.0 L·min^(-1))。结果:亚甘油三油酸酯、1,2-二亚油酸-3-油酸甘油酯、1,2-二亚油酸-3-棕榈酸甘油酯、1,2-二油酸-3-亚油酸甘油酯、1-棕榈酸-2-油酸-3-亚油酸甘油酯、甘油三油酸酯、1,2-二油酸-3-棕榈酸甘油酯、1,2-二油酸-3-硬脂酸甘油酯的线性范围分别为0.029~0.861μg(r^2=0.999 3)、0.147~4.404μg(r^2=0.998 8)、0.051~1.523μg(r^2=0.999 4)、0.280~8.388μg(r^2=0.999 3)、0.242~7.263μg(r^2=0.998 9)、0.613~18.40μg(r^2=0.998 9)、0.342~10.25μg(r^2=0.999 0)、0.069~2.075μg(r^2=0.999 5);加样回收率分别为100.3%、92.9%、102.2%、93.9%、94.2%、104.1%、99.6%和100.7%,RSD分别为4.6%、2.5%、3.0%、3.3%、3.1%、1.8%、2.9%和4.3%。测定了4批未破壁灵芝孢子粉和21批破壁灵芝孢子粉中油脂类成分的含量,结果 4批未破壁灵芝孢子粉均检出上述8个油脂类成分;21批破壁灵芝孢子粉中上述8个油脂类成分含量分别为1.9~6.9、6.2~18.2、1.9~5.8、18.5~46.1、8.3~30.2、30.9~79.0、34.2~123.3和5.6~17.4 mg·g^(-1)。结论:该方法适用于灵芝孢子粉的质量控制与评价。

Objective：To establish a high performance liquid chromatography method with evaporative light scattering detector（HPLC-ELSD）for determination of eight lipin components in Ganoderma lucidum spore powder.Methods：The chromatographic separation was performed on an ACCHROM Unitary-C_（18） column（4.6 mm×250 mm,5 μm）with the mobile phase of acetonitrile-isopropanol（51∶49）.The flow rate was 1.0mL·min（-1） at 30 ℃ with the detection by ELSD（drift tube temperature was 105 ℃ and gas flow rate was 2.0 L·min（-1））. Results：The calibration curve was linear for trilinolein,1,2-linolein-3-olein,1,2-linolein-3-palmitin,1,2-olein-3-linolein,1-palmitin-2-olein-3-linolein,triolein,1,2-olein-3-palmitin and 1,2-olein-3-stearin in the ranges of 0.029-0.861 μg（r-2=0.999 3）,0.147-4.404 μg（r-2=0.998 8）,0.051（-1）.523 μg（r-2=0.999 4）,0.280-8.388 μg（r-2=0.999 3）,0.242-7.263 μg（r-2=0.998 9）,0.613（-1）8.40 μg（r-2=0.998 9）,0.342（-1）0.25 μg（r-2=0.999 0）,and 0.069-2.075 μg（r-2=0.999 5）,respectively.The contents of above eight lipin components were determined in 4 batches of sporoderm-unbroken Ganoderma lucidum spore powder samples and 21 batches of sporoderm-broken Ganoderma lucidum spore powder samples.All the eight components were not detected in 4 batches of sporoderm-unbroken Ganoderma lucidum spore powder.The contents of eight lipin components in 21 batches of sporoderm-broken Ganoderma lucidum spore powder were 1.9-6.9 mg·g（-1）,6.2（-1）8.2 mg·g（-1）,1.9-5.8 mg·g（-1）,18.5-46.1 mg·g（-1）,8.3-30.2 mg·g（-1）,30.9-79.0 mg·g（-1）,34.2（-1）23.3 mg·g（-1）,and 5.6（-1）7.4 mg·g（-1）.Conclusion：The method can be used for quality control of Ganoderma lucidum spore powder.