HPLC-DAD-ELSD测定红古豆醇酯含量和有关物质方法的建立

Determination of the Content and the Related Compounds in Cuscohygrinolis α-Acetylbenzoacetate by HPLC-DAD-ELSD

目的建立二极管阵列检测器和蒸发光散射检测器联用高效液相色谱测定红古豆醇酯中红古豆醇和乙酰苦杏仁酸等有关物质及含量的方法。方法采用Waters symmetry C18柱(4.6 mm×150 mm,5μm);以甲醇-0.25%五氟丙酸(含30 mmol.L-1甲酸铵)(45∶55)为流动相;紫外检测器(检测波长219 nm)和蒸发光散射检测器联用检测,柱温为室温。结果红古豆醇、乙酰苦杏仁酸和红古豆醇酯能够达到很好分离。其线性范围分别为0.016 32～0.163 2,0.005 65～0.113 g.L-1,和0.228 2～2.282 g.L-1;平均回收率分别为100.1%,101.2%和99.6%,结论本法简单、准确、快速,可用于红古豆醇酯中红古豆醇、乙酰苦杏仁酸等有关物质的检查及含量测定。

OBJECTIVE To establish a HPLC-DAD-ELSD method for the deter mination of the content of cuscohygrinol, acetylmandelic acid and other related compounds in cuscohygrinolis α-acetylbenzoacetate. METHODS The HPLC method was conducted on a Waters symmetry C18 column （4.6 min× 150 mm, 5 μm） and coupled with ELSD and DAD detector at 219 nm. The mobile phase consisted of methanol-0.25% of pentafluoropropionic acid （contains 30 mmol·L^-1 of ammonium formate）, and the column temperature was at room temperature. RESULTS A good resolution was obtained among cuscohygrinol, acetylmandelic acid, cuscohygrinolis α-acetylbenzoacetate and other related compound. The linear ranges of cuscohygrinol, aeetylmandelic acid and cuscohygrinolis α-acetylbenzoacetate were 0.016 32-0.163 2, 0.005 65-0.113 and 0.228 2-2.282 g·L^-1, respectively. The average recovery of cuscohygrinol, acetylmandelic acid and cuscohygrinolis α-acetylbenzoacetate were 100.1%, 101.2% and 99.6% respectively. CONCLUSION A simple, accurate and sensitive HPLC-DAD-ELSD method to determine the content of cuscohygrinol, acetylmandelic acid and other related compounds in cuscohygrinolis ct-acetylbenzoacetate was established.