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

摘要/Abstract

摘要：

建立了高效液相色谱（HPLC）法同时检测丹芝防晒霜SFP50中11种成分含量。以黄芩苷为含量参照物，乙腈-体积分数0.1%磷酸为流动相，检测波长为205和280 nmn，分别采用外标法和高效液相色谱一测多评法（HPLC-QAMS）同时测定12批丹芝防晒霜SFP50中羟基积雪草苷、积雪草苷、羟基积雪草酸、积雪草酸、虎杖苷、白藜芦醇、黄芩苷、汉黄芩苷、甘草苷、甘草酸、光甘草定的含量，对比两种方法的结果差异，验证HPLC-QAMS的适用性。结果表明，11种成分各线性范围良好，相关系数（R）均大于0.999，11种成分的平均加样回收率为96.90%~100.16%，RSD均小于2.0%。两种方法测得的丹芝防晒霜SFP50中11种成分的含量差异均无统计学意义（P>0.05）。以黄芩苷为含量参照物建立的相对校正因子重现性好。

关键词: 防晒霜, 高效液相色谱法, 含量测定

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

中图分类号:

TQ658

冯利,邹柏松. 高效液相色谱法同时测定丹芝防晒霜SFP50中11种成分含量[J]. 日用化学工业（中英文）, 2023, 53(8): 968-975.

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.

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参考文献 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