高效液相色谱法同时测定丹芝防晒霜SFP50中11种成分含量

doi:10.3969/j.issn.2097-2806.2023.08.014

Abstract

Abstract:

A high performance liquid chromatography （HPLC） method was established to simultaneously detect the contents of 11 components in Danzhi Fangshaishuang SFP50, and the feasibility and accuracy of the established method were verified. Baicalin was used as the reference substance and acetonitrile-0.1% phosphoric acid was used as the mobile phase, with the detecting wavelength of 205 nm and 280 nm. The contents of madecassoside, asiaticoside, madecassic acid, asiatic acid, polydatin, resveratrol, baicalin, wogonoside, liquiritin, glycyrrhizic acid and glabridin in 12 batches of Danzhi Fangshaishuang SFP50 were determined by external standard method and HPLC-quantitative analysis of multi-components by single-marker （QAMS） method, respectively, and the difference between the results from the two methods was compared to verify the serviceability of HPLC-QAMS method. The results show that the linear ranges of the 11 components are good, and the correlation coefficients are greater than 0.999. The average recoveries of 11 components are 96.90%-100.16%, and RSD is less than 2.0%. There is no statistical significance of 11 components in Danzhi Fangshaishuang SFP50 determined by external standard method and HPLC-QAMS method （P>0.05）. The relative correlation factors established with baicalin as the internal reference substance have good reproducibility.

Key words: sunscreen, high performance liquid chromatography, content determination

CLC Number:

TQ658

Feng Li,Zou Baisong. Simultaneous determination of 11 components in Danzhi Fangshaishuang SFP50 by HPLC[J].China Surfactant Detergent & Cosmetics, 2023, 53(8): 968-975.

Figures/Tables 8

Fig. 1

Tab. 1

Tab. 2

Tab. 3

Tab. 4

Tab. 5

Tab. 6

Tab. 7

References 17

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序号	成分	回归方程	线性范围（μg/mL）	r
1	羟基积雪草苷	Y=5.050 6×10⁶X+1 172.2	1.77~ 88.50	0.999 7
2	积雪草苷	Y=3.563 6×10⁶X-374.7	1.16~ 58.00	0.999 3
3	羟基积雪草酸	Y=3.202 1×10⁶X-1 306.1	0.95~ 47.50	0.999 7
4	积雪草酸	Y=1.463 7×10⁶X+415.8	0.41~ 20.50	0.999 4
5	虎杖苷	Y=1.802 8×10⁶X+1 040.1	0.48~ 24.00	0.999 6
6	白藜芦醇	Y=2.283 9×10⁶X+205.2	0.57~ 28.50	0.999 3
7	黄芩苷	Y=2.932 0×10⁶X-952.3	6.45~322.50	0.999 4
8	汉黄芩苷	Y=4.747 7×10⁶X+1 218.9	1.69~ 84.50	0.999 6
9	甘草苷	Y=2.709 3×10⁶X+348.7	0.78~ 39.00	0.999 3
10	甘草酸	Y=3.326 1×10⁶X-1 767.8	3.80~190.00	0.999 5
11	光甘草定	Y=4.249 0×10⁶X+737.4	1.47~ 73.50	0.999 4

混合对照品溶液	?
混合对照品溶液	羟基积雪草苷	积雪草苷	羟基积雪草酸	积雪草酸	虎杖苷	白藜芦醇	汉黄芩苷	甘草苷	甘草酸	光甘草定
1	0.587 5	0.814 7	0.942 3	2.001 3	1.641 3	1.269 5	0.635 5	1.081 3	0.886 0	0.690 8
2	0.585 8	0.812 8	0.915 4	2.000 4	1.641 0	1.272 7	0.617 1	1.065 8	0.885 5	0.690 8
3	0.592 3	0.813 2	0.939 4	2.004 2	1.637 1	1.268 9	0.620 6	1.064 5	0.886 3	0.684 2
4	0.585 9	0.819 7	0.925 1	1.992 2	1.639 4	1.281 2	0.620 6	1.078 8	0.881 8	0.687 0
5	0.570 2	0.831 7	0.898 4	2.006 2	1.601 1	1.294 2	0.611 7	1.093 8	0.878 5	0.693 9
6	0.581 7	0.821 7	0.917 8	2.002 7	1.628 8	1.282 4	0.618 2	1.080 8	0.881 9	0.689 6
平均值	0.583 9	0.819 0	0.923 1	2.001 2	1.631 5	1.278 1	0.620 6	1.077 5	0.883 4	0.689 4
RSD/%	1.28	0.88	1.77	0.24	0.96	0.77	1.29	1.01	0.35	0.49

仪器型号	色谱柱	?
仪器型号	色谱柱	羟基积雪草苷	积雪草苷	羟基积雪草酸	积雪草酸	虎杖苷	白藜芦醇	汉黄芩苷	甘草苷	甘草酸	光甘草定
Agilent 1260	Hypersil BDS C₁₈	0.574 2	0.811 7	0.912 6	2.000 0	1.623 7	1.261 9	0.611 3	1.064 2	0.879 1	0.682 6
	Diamonsil C₁₈	0.583 7	0.818 5	0.922 8	2.001 1	1.631 2	1.277 3	0.620 1	1.076 5	0.883 2	0.689 1
	Waters ODS C₁₈	0.589 2	0.827 6	0.948 1	2.014 2	1.656 8	1.288 2	0.629 8	1.089 1	0.889 6	0.695 4
Primaide 1430	Hypersil BDS C₁₈	0.572 4	0.810 9	0.911 4	1.998 7	1.620 5	1.260 7	0.610 2	1.063 3	0.877 2	0.681 9
	Diamonsil C₁₈	0.581 7	0.817 2	0.921 9	2.000 5	1.631 1	1.276 4	0.619 6	1.075 7	0.882 5	0.688 5
	Waters ODS C₁₈	0.588 6	0.826 4	0.946 3	2.013 9	1.644 8	1.286 9	0.627 5	1.087 3	0.885 1	0.691 6
平均值		0.581 6	0.818 7	0.927 2	2.004 7	1.634 7	1.275 2	0.619 7	1.076 0	0.882 8	0.688 2
RSD/%		1.22	0.86	1.75	0.36	0.84	0.93	1.30	1.02	0.50	0.76

流速/ （mL/min）	羟基积雪草苷	?
流速/ （mL/min）	羟基积雪草苷	积雪草苷	羟基积雪草酸	积雪草酸	虎杖苷	白藜芦醇	汉黄芩苷	甘草苷	甘草酸	光甘草定
0.8	0.574 3	0.813 2	0.904 2	1.998 7	1.623 8	1.268 5	0.613 5	1.065 9	0.879 2	0.684 2
1.0	0.583 6	0.818 5	0.921 9	2.000 4	1.632 7	1.276 2	0.621 9	1.078 1	0.883 7	0.689 6
1.2	0.589 1	0.827 3	0.937 6	2.011 2	1.656 1	1.289 7	0.627 4	1.089 2	0.887 5	0.691 7
平均值	0.582 3	0.819 7	0.921 2	2.003 4	1.637 5	1.278 1	0.620 9	1.077 7	0.883 5	0.688 5
RSD/%	1.28	0.87	1.81	0.34	1.02	0.84	1.13	1.08	0.47	0.56

柱温/℃	?
柱温/℃	羟基积雪草苷	积雪草苷	羟基积雪草酸	积雪草酸	虎杖苷	白藜芦醇	汉黄芩苷	甘草苷	甘草酸	光甘草定
25	0.575 6	0.812 4	0.906 5	1.996 5	1.621 6	1.267 9	0.614 3	1.064 2	0.878 5	0.685 7
30	0.584 2	0.818 1	0.922 3	2.001 7	1.631 1	1.278 5	0.621 5	1.078 3	0.884 2	0.689 8
35	0.588 9	0.828 3	0.939 6	2.012 4	1.658 2	1.286 4	0.629 8	1.087 9	0.888 3	0.692 1
平均值	0.582 9	0.819 6	0.922 8	2.003 5	1.637 0	1.277 6	0.621 9	1.076 8	0.883 7	0.689 2
RSD/%	1.16	0.98	1.79	0.41	1.16	0.73	1.25	1.11	0.56	0.47

Simultaneous determination of 11 components in Danzhi Fangshaishuang SFP50 by HPLC

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仪器型号	色谱柱	t
仪器型号	色谱柱	羟基积雪草苷	积雪草苷	羟基积雪草酸	积雪草酸	虎杖苷	白藜芦醇	汉黄芩苷	甘草苷	甘草酸	光甘草定
Agilent 1260	Hypersil BDS C₁₈	0.368 4	0.454 1	0.554 9	0.652 6	0.825 6	0.911 3	1.108 3	1.188 0	1.276 7	1.359 4
	Diamonsil C₁₈	0.369 2	0.455 3	0.555 6	0.653 4	0.827 0	0.912 7	1.119 6	1.199 2	1.275 2	1.364 2
	Waters ODS C₁₈	0.379 8	0.467 9	0.569 1	0.662 9	0.839 8	0.929 5	1.128 1	1.216 7	1.299 6	1.397 8
Primaide 1430	Hypersil BDS C₁₈	0.361 1	0.450 7	0.551 5	0.649 8	0.820 1	0.904 1	1.100 4	1.173 5	1.264 3	1.343 6
	Diamonsil C₁₈	0.368 7	0.455 2	0.554 7	0.652 1	0.821 3	0.911 4	1.118 7	1.197 2	1.274 1	1.362 7
	Waters ODS C₁₈	0.376 9	0.465 4	0.568 9	0.661 7	0.838 9	0.927 8	1.127 5	1.215 4	1.298 5	1.396 3
平均值		0.370 7	0.458 1	0.559 1	0.655 4	0.828 8	0.916 1	1.117 1	1.198 3	1.281 4	1.370 7
RSD/%		1.81	1.50	1.39	0.84	1.04	1.11	0.98	1.37	1.12	1.58

成分	含量/（mg/g）
成分	黄芩苷	羟基积雪草苷			积雪草苷			羟基积雪草酸			积雪草酸			虎杖苷
方法	ESM	ESM	QAMS	RSD/%	ESM	QAMS	RSD/%	ESM	QAMS	RSD/%	ESM	QAMS	RSD/%	ESM	QAMS	RSD/%
S1	0.918	0.181	0.185	1.09	0.129	0.131	0.77	0.107	0.108	0.47	0.039	0.040	1.27	0.052	0.053	0.95
S2	0.923	0.219	0.213	1.39	0.162	0.158	1.25	0.104	0.102	0.97	0.045	0.044	1.12	0.048	0.049	1.03
S3	0.931	0.198	0.195	0.76	0.149	0.147	0.68	0.105	0.103	0.96	0.044	0.043	1.15	0.056	0.057	0.88
S4	0.911	0.215	0.210	1.18	0.153	0.151	0.66	0.095	0.094	0.53	0.040	0.039	1.27	0.055	0.054	0.92
S5	0.907	0.210	0.207	0.72	0.133	0.132	0.38	0.097	0.096	0.52	0.040	0.041	1.23	0.053	0.052	0.95
S6	0.925	0.169	0.167	0.60	0.137	0.136	0.37	0.092	0.090	1.10	0.041	0.042	1.20	0.051	0.050	0.99
S7	0.938	0.205	0.202	0.74	0.154	0.151	0.98	0.091	0.092	0.55	0.039	0.038	1.30	0.057	0.058	0.87
S8	0.933	0.207	0.206	0.24	0.142	0.140	0.71	0.115	0.118	1.29	0.037	0.036	1.37	0.056	0.055	0.90
S9	0.926	0.176	0.172	1.15	0.145	0.147	0.68	0.104	0.102	0.97	0.035	0.034	1.45	0.048	0.047	1.05
S10	0.915	0.168	0.169	0.30	0.146	0.145	0.34	0.102	0.101	0.49	0.036	0.035	1.41	0.047	0.046	1.08
S11	0.909	0.181	0.183	0.55	0.124	0.122	0.81	0.115	0.117	0.86	0.038	0.037	1.33	0.046	0.045	1.10
S12	0.904	0.182	0.179	0.83	0.128	0.125	1.19	0.107	0.105	0.94	0.034	0.035	1.45	0.049	0.048	1.03