HPLC-ELSD法测定破壁灵芝孢子粉中8个油脂类成分的含量

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-C₁₈ 色谱柱（250 mm×4.6 mm，5 μm），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0.029~0.861 μg（r²=0.999 3）、0.147~4.404 μg（r²=0.998 8）、0.051~1.523 μg（r²=0.999 4）、0.280~8.388 μg（r²=0.999 3）、0.242~7.263 μg（r²=0.998 9）、0.613~18.40μg（r²=0.998 9）、0.342~10.25 μg（r²=0.999 0）、0.069~2.075 μg（r²=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-C₁₈ column (4.6 mm×250 mm,5 μm)with the mobile phase of acetonitrile-isopropanol(51:49). The flow rate was 1.0 mL·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(r²=0.999 3),0.147-4.404 μg(r²=0.998 8),0.051-1.523 μg(r²=0.999 4),0.280-8.388 μg(r²=0.999 3), 0.242-7.263 μg(r²=0.998 9),0.613-18.40 μg(r²=0.998 9),0.342-10.25 μg(r²=0.999 0),and 0.069-2.075 μg(r²=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^-1,6.2-18.2 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^-1,34.2-123.3 mg·g^-1,and 5.6-17.4 mg·g^-1. Conclusion: The method can be used for quality control of Ganoderma lucidum spore powder.

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