HPLC-QAMS法同时测定何首乌防脱育发精华液中9种成分含量

doi:10.3969/j.issn.2097-2806.2023.07.015

Abstract

Abstract:

The study aimed to establish an HPLC-QAMS method for simultaneous quantitation of nine effective components in Polygonum Multiflorum Fangtuoyufa Jinghuaye, and to verify the feasibility and accuracy of the method. Quercitrin was used as the reference substance and methanol-0.1% phosphoric acid was used as the mobile phase. The contents of emodin, physcion, myricitrin, quercitrin, myricetin, quercetin, kaempferol, amentoflavone and hinokiflavone in 12 batches of Polygonum Multiflorum Fangtuoyufa Jinghuaye were determined by external standard method and HPLC-QAMS method, respectively, and the difference between the results of the two methods was compared to verify the serviceability of HPLC-QAMS method. The results show that the linear ranges of the nine components are good, the correlation coefficients are greater than 0.999, the limits of detection （LOD） are 0.027-0.151 µg/mL, and the limits of quantification are 0.076-0.449 µg/mL. The relative correlation factors are 0.753 7, 0.836 9, 1.019 2, 2.991 3, 1.687 5, 2.236 9, 1.096 3 and 1.249 3 for emodin, physcion, myricitrin, myricetin, quercetin, kaempferol, amentoflavone and hinokiflayone, respectively. There is no significant difference in the content of 9 components in Polygonum Multiflorum Fangtuoyufa Jinghuaye determined by the two methods （P>0.05）. The relative correlation factors established with quercitrin as the internal reference substance have good reproducibility. The HPLC-QAMS method can be used for the quality evaluation of nine effective components in Polygonum Multiflorum Fangtuoyufa Jinghuaye.

Key words: Polygonum Multiflorum Fangtuoyufa Jinghuaye, HPLC-QAMS, content determination, relative correlation factor

CLC Number:

TQ658

Liu Ying, Lin Min, Dai Sirui. Simultaneous determination of nine effective components in Polygonum Multif lorum Fangtuoyufa Jinghuaye by HPLC-QAMS[J].China Surfactant Detergent & Cosmetics, 2023, 53(7): 841-848.

Figures/Tables 8

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References 18

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成分	回归方程	线性范围/（μg/mL）	r	检出限/（μg/mL）	定量限/（μg/mL）
大黄素	Y=2.776 2×10⁶X-806.3	0.96~192.00	0.999 5	0.107	0.304
大黄素甲醚	Y=2.485 6×10⁶X+1 017.5	0.68~136.00	0.999 2	0.084	0.257
杨梅苷	Y=2.041 9×10⁶X+663.1	1.35~270.00	0.999 1	0.151	0.449
槲皮苷	Y=2.093 2×10⁶X-1 018.0	1.57~314.00	0.999 6	0.132	0.375
杨梅素	Y=6.971 5×10⁵X-471.2	0.26~52.00	0.999 4	0.027	0.076
槲皮素	Y=1.236 5×10⁶X+753.8	0.39~78.00	0.999 1	0.043	0.127
山柰酚	Y=9.364 4×10⁵X-621.3	0.32~64.00	0.999 5	0.051	0.148
穗花杉双黄酮	Y=1.913 7×10⁶X+1 005.6	0.59~118.00	0.999 2	0.065	0.201
扁柏双黄酮	Y=1.671 5×10⁶X+1 022.9	0.46~92.00	0.999 7	0.039	0.112

混合对照品溶液	?
混合对照品溶液	大黄素	大黄素甲醚	杨梅苷	杨梅素	槲皮素	山柰酚	穗花杉双黄酮	扁柏双黄酮
1	0.758 2	0.827 4	1.003 5	2.970 1	1.690 4	2.250 2	1.120 9	1.247 1
2	0.747 5	0.816 8	1.001 9	2.976 1	1.675 6	2.238 2	1.078 1	1.249 9
3	0.752 0	0.855 1	1.046 8	2.964 9	1.695 0	2.234 3	1.104 9	1.246 3
4	0.756 1	0.833 6	1.016 7	3.005 4	1.671 9	2.247 4	1.088 7	1.257 9
5	0.757 8	0.856 9	1.022 8	3.074 1	1.714 9	2.203 8	1.088 7	1.241 4
6	0.750 8	0.831 8	1.023 4	2.957 5	1.677 4	2.247 7	1.096 6	1.253 4
平均值	0.753 7	0.836 9	1.019 2	2.991 3	1.687 5	2.23	1.096 3	1.249 3
RSD/%	0.57	1.90	1.61	1.46	0.95	0.78	1.37	0.46

仪器	色谱柱	?
仪器	色谱柱	大黄素	大黄素甲醚	杨梅苷	杨梅素	槲皮素	山柰酚	穗花杉双黄酮	扁柏双黄酮
LC-20AC	Agilent ZORBAX ODS C₁₈	0.750 2	0.822 1	1.001 6	2.956 3	1.671 6	2.214 3	1.079 2	1.236 7
	Welch UltimateLP-C₁₈	0.753 7	0.835 4	1.019 7	2.990 6	1.685 2	2.239 2	1.095 1	1.248 2
	Waters ODS C₁₈	0.759 6	0.857 9	1.037 9	3.035 2	1.699 7	2.258 7	1.114 9	1.253 6
Waters e2695	Agilent ZORBAX ODS C₁₈	0.748 2	0.821 5	1.000 4	2.954 3	1.670 1	2.212 4	1.078 7	1.234 6
	Welch UltimateLP-C₁₈	0.752 4	0.832 3	1.018 2	2.988 7	1.684 4	2.238 1	1.094 4	1.246 4
	Waters ODS C₁₈	0.758 8	0.854 1	1.036 5	3.034 5	1.698 9	2.257 6	1.113 2	1.251 8
平均值		0.753 8	0.837 2	1.019 1	2.993 3	1.685 0	2.236 4	1.095 9	1.245 2
RSD/%		0.61	1.86	1.59	1.19	0.76	0.88	1.44	0.63

流速/ （mL/min）	?
流速/ （mL/min）	大黄素	大黄素甲醚	杨梅苷	杨梅素	槲皮素	山柰酚	穗花杉双黄酮	扁柏双黄酮
0.8	0.750 6	0.820 3	1.001 6	2.950 1	1.671 3	2.216 3	1.080 2	1.241 6
1.0	0.753 2	0.830 7	1.014 3	2.992 6	1.688 5	2.227 6	1.096 1	1.249 7
1.2	0.759 7	0.851 2	1.036 1	3.027 9	1.699 7	2.249 8	1.107 8	1.256 2
平均值	0.754 5	0.834 1	1.017 3	2.990 2	1.686 5	2.231 2	1.094 7	1.249 2
RSD/%	0.62	1.89	1.72	1.30	0.85	0.76	1.27	0.59

柱温/℃	?
柱温/℃	大黄素	大黄素甲醚	杨梅苷	杨梅素	槲皮素	山柰酚	穗花杉双黄酮	扁柏双黄酮
25	0.748 1	0.820 0	1.006 2	2.952 4	1.670 3	2.214 6	1.078 3	1.241 3
30	0.754 3	0.837 1	1.019 6	2.992 7	1.685 9	2.237 8	1.097 3	1.249 6
35	0.758 4	0.849 8	1.037 9	3.029 6	1.699 5	2.258 1	1.111 5	1.254 7
平均值	0.753 6	0.835 6	1.021 2	2.991 6	1.685 2	2.236 8	1.095 7	1.248 5
RSD/%	0.69	1.79	1.56	1.29	0.87	0.97	1.52	0.54

Simultaneous determination of nine effective components in Polygonum Multif lorum Fangtuoyufa Jinghuaye by HPLC-QAMS

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成分	方法	含量测定结果/（mg/g）												P
成分	方法	S1	S2	S3	S4	S5	S6	S7	S8	S9	S10	S11	S12	P
槲皮苷	ESM	0.178	0.181	0.176	0.179	0.180	0.177	0.176	0.175	0.176	0.178	0.180	0.174	—
大黄素	ESM	0.107	0.109	0.113	0.102	0.117	0.109	0.116	0.101	0.103	0.105	0.108	0.118	0.827
大黄素	QAMS	0.109	0.107	0.116	0.105	0.104	0.112	0.119	0.103	0.105	0.108	0.111	0.115	0.827
大黄素甲醚	ESM	0.081	0.082	0.081	0.082	0.080	0.083	0.081	0.082	0.083	0.080	0.082	0.083	0.139
大黄素甲醚	QAMS	0.083	0.084	0.083	0.081	0.082	0.084	0.083	0.080	0.082	0.081	0.084	0.082	0.139
杨梅苷	ESM	0.141	0.148	0.139	0.145	0.140	0.146	0.138	0.147	0.142	0.136	0.149	0.143	0.812
杨梅苷	QAMS	0.142	0.144	0.142	0.147	0.142	0.145	0.141	0.144	0.140	0.140	0.145	0.146	0.812
杨梅素	ESM	0.029	0.028	0.029	0.030	0.028	0.031	0.030	0.029	0.031	0.028	0.027	0.031	0.131
杨梅素	QAMS	0.030	0.029	0.030	0.031	0.029	0.030	0.031	0.030	0.032	0.029	0.028	0.032	0.131
槲皮素	ESM	0.043	0.043	0.044	0.042	0.041	0.044	0.043	0.042	0.045	0.043	0.044	0.042	0.143
槲皮素	QAMS	0.044	0.045	0.043	0.043	0.042	0.045	0.042	0.043	0.046	0.044	0.045	0.043	0.143
山柰酚	ESM	0.031	0.030	0.032	0.033	0.029	0.030	0.031	0.032	0.031	0.030	0.029	0.032	0.338
山柰酚	QAMS	0.032	0.031	0.033	0.034	0.030	0.031	0.030	0.031	0.032	0.031	0.030	0.031	0.338
穗花杉双黄酮	ESM	0.068	0.069	0.067	0.068	0.069	0.066	0.070	0.069	0.068	0.067	0.068	0.069	0.380
穗花杉双黄酮	QAMS	0.069	0.068	0.069	0.067	0.068	0.067	0.071	0.070	0.069	0.068	0.069	0.068	0.380
扁柏双黄酮	ESM	0.052	0.051	0.053	0.052	0.053	0.053	0.054	0.052	0.051	0.050	0.052	0.054	0.170
扁柏双黄酮	QAMS	0.053	0.052	0.054	0.053	0.054	0.052	0.053	0.053	0.052	0.051	0.053	0.055	0.170

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仪器	t
仪器	色谱柱	大黄素	大黄素甲醚	杨梅苷	杨梅素	槲皮素	山柰酚	穗花杉双黄酮	扁柏双黄酮
LC-20AC	Agilent ZORBAX ODS C₁₈	0.571 4	0.695 8	0.907 4	1.179 9	1.338 6	1.547 6	1.743 4	2.087 3
	Welch UltimateLP-C₁₈	0.576 2	0.701 6	0.908 1	1.178 1	1.339 1	1.548 3	1.740 3	2.089 7
	Waters ODS C₁₈	0.581 7	0.708 3	0.924 3	1.199 3	1.368 5	1.569 8	1.769 7	2.119 5
Waters e2695	Agilent ZORBAX ODS C₁₈	0.572 1	0.681 5	0.891 7	1.161 7	1.312 2	1.520 7	1.728 9	2.064 2
	Welch UltimateLP-C₁₈	0.574 4	0.693 7	0.906 6	1.175 2	1.323 7	1.542 2	1.731 3	2.081 4
	Waters ODS C₁₈	0.580 6	0.707 4	0.923 9	1.195 5	1.366 8	1.567 5	1.768 5	2.117 6
平均值		0.576 1	0.698 0	0.910 3	1.181 6	1.341 5	1.549 3	1.747 0	2.093 3
RSD/%		0.75	1.44	1.35	1.17	1.69	1.16	1.03	1.03