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一测多评法同时测定木瓜中5种五环三萜类成分的含量
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| 篇名： | 一测多评法同时测定木瓜中5种五环三萜类成分的含量 |
| TITLE： | Simultaneous determination of 5 kinds of pentacyclic triterpenoids in Chaenomeles speciosa by quantitative analysis of multi-components by single-marker |
| 摘要： | 目的 建立同时测定木瓜中3-O-乙酰坡模醇酸等5种五环三萜类成分含量的方法，并分析不同产地、不同炮制工艺木瓜的含量差异。方法以高效液相色谱法为检测手段，色谱柱为COSMOSIL5C18-MS-Ⅱ，流动相为乙腈-0.005mol/L磷酸氢二铵溶液（用磷酸调pH至6.5）（70︰30，V/V），流速为1.0mL/min，柱温为30℃，检测波长为210nm，进样量为20μL。以齐墩果酸为内参物，结合一测多评法，对3-O-乙酰坡模醇酸等4种五环三萜类成分含量进行测定，并与外标法进行比较；同时，对不同产地、不同炮制加工工艺木瓜中齐墩果酸与熊果酸的总含量和5种成分的总含量进行比较。结果3-O-乙酰坡模醇酸、白桦脂酸、齐墩果酸、熊果酸、3-O-乙酰熊果酸检测质量浓度的线性范围分别为4.06～81.2、2.12～42.4、9.62～192.3、7.77～155.4、4.21～84.1μg/mL（R2＞0.999）；精密度、重复性、稳定性（24h）试验的RSD均小于3%；平均加样回收率为98.29%～101.38%（RSD＜3%，n＝6）。一测多评法测得3-O-乙酰坡模醇酸、白桦脂酸、熊果酸、3-O-乙酰熊果酸的含量分别为0.023%～0.060%、0.044%～0.528%、0.101%～0.368%、0.067%～0.221%，与外标法所测结果的相对偏差均小于8%。同一产地鲜切工艺加工木瓜中齐墩果酸与熊果酸的总含量和5种成分的总含量均高于传统工艺加工木瓜，且重庆黔江产木瓜中5种成分的总含量显著高于其他产地（P＜0.05）。结论建立了同时测定木瓜中3-O-乙酰坡模醇酸、白桦脂酸、齐墩果酸、熊果酸、3-O-乙酰熊果酸含量的一测多评法，该方法简便、快速、准确。重庆黔江产木瓜中5种成分的总含量较高，且同一产地鲜切工艺加工木瓜总含量高于传统工艺加工木瓜。 |
| ABSTRACT： | OBJECTIVE To establish a method for simultan eous determination of 5 kinds of pentacyclic triterpenoids as 3-O- acetyl-pomolic acid in Chaenomeles speciosa ，and to analyze the difference in the contents of C. speciosa from different producing areas by different processing technologies . METHODS HPLC method was adopted . The determination was performed on COSMOSIL 5 C18-MS-Ⅱ column with mobile phase consisted of acetonitrile -0.005 mol/L ammonium dihydrogen phosphate solution （pH value adjusted to 6.5 with phosphoric acid ）（70∶30，V/V）at the flow rate of 1.0 mL/min. The column temperature was set at 30 ℃. The detection wavelength was set at 210 nm，and sample size was 20 μL. The contents of the other four pentacyclic triterpenoids were calculated according to quantitative analysis of multi -components by single -marker（QAMS）using oleanolic acid as internal reference . The results were compared with those determined by external standard method . The total content of oleanolic acid and ursolic acid ，the total content of 5 components in C. speciosa from different producing areas and different processing technologies were compared . RESULTS The linear range of 3-O-acetyl-pomolic acid ，betulinic acid ，oleanolic acid ，ursolic acid and 3-O-acetyl ursolic acid were 4.06-81.2，2.12-42.4，9.62-192.3，7.77-155.4，4.21-84.1 μg/mL，respectively（R2＞0.999）. RSDs of precision ，reproducibility and stability （24 h）tests were all lower than 3%. The average recoveries were 98.29%-101.38% （RSDs＜3%，n＝6）. The mass fraction of 3-O-acetyl-pomolic acid ，betulinic acid ，ursolic acid and 3-O-acetyl ursolic acid measured by QAMS w ere 0.023%-0.060%，0.044%-0.528%，0.101%-0.368%，0.067%-0.221%，respectively；the deviations from the results measured by external standard method were all within 8%. The total content of oleanolic acid and ursolic acid， the total content of 5 components in C. speciosa processed by fresh -cut technology from the same producing area were higher than those in C. speciosa processed by traditional technology ，and the total content of 5 components in C. speciosa from Chongqing Qianjiang were significantly higher than those from other producing areas （P＜0.05）. CONCLUSIONS QAMS method is established for the simultaneous determination of 3-O-acetyl-pomolic acid ，betulinic acid ，oleanolic acid ，ursolic acid and 3-O-acetyl ursolic acid in C. speciosa. Established method is simple ，rapid and accurate . The total content of 5 components in C. speciosa produced in Chongqing Qianjiang is higher ，and the total content of C. speciosa processed by fresh -cut technology from the same origin is higher than C. speciosa processed by traditional technology . |
| 期刊： | 2022年第33卷第20期 |
| 作者： | 张亭亭，胡浩宁，李平媛，黄永梅，汪鋆植，唐海明，尹永红 |
| AUTHORS： | ZHANG Tingting，HU Haoning，LI Pingyuan，HUANG Yongmei，WANG Junzhi，TANG Haiming，YIN Yonghong |
| 关键字： | 木瓜；五环三萜类成分；一测多评法；含量测定 |
| KEYWORDS： | Chaenomeles speciosa ；pentacyclic triterpenoids ；quantitative analysis of multi -components by single -marker； |
| 阅读数： | 185 次 |
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