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;
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