高效液相色谱法测定口洁含漱液中13种化学成分的含量

doi:10.3969/j.issn.2097-2806.2023.10.016

Abstract

Abstract:

The study aimed to develop an high performance liquid chromatography （HPLC） method for the determination of neochlorogenic acid, chlorogenic acid, caffeic acid, luteolin-7-O-glucoside, 3,5-dicaffeoylquinic acid, 4,5-dicaffeoylquinic acid, luteolin, apigenin, loganin, sweroside, secoxyloganin; （R, S）-goitrin and clemastanin B in Koujie gargle. Separation was carried out using Waters Symmetry C₁₈（250 mm×4.6 mm, 5 μm） with mobile phase of acetonitrile-0.3% phosphoric acid in gradient elution. The detection wavelength was set at 348 nm, 240 nm and 224 nm. The flow rate was 1.0 mL/min, and the column temperature was 30 ℃. The results show that the linear relationship of 13 chemical components in Koujie gargle is good （r≥0.999 1）, the average recovery ranges from 96.92% to 100.11%, and the RSD ranges from 0.53% to 1.58%. The established HPLC wavelength switching method is accurate which can be used for the quality control of Koujie gargle.

Key words: Koujie gargle, high performance liquid chromatography, oral care products, content determination

CLC Number:

TQ658

Wu Xiaoyan, Song Faxiang. Determination of 13 chemical components in Koujie gargle by HPLC[J].China Surfactant Detergent & Cosmetics, 2023, 53(10): 1233-1240.

Figures/Tables 4

Fig. 1

Tab. 1

Tab. 2

Sample recovery test results （n=9）"

成分	样品中含量/mg	加入量/mg	测得量/mg	回收率/%	平均加样回收率/%	RSD/%
新绿原酸	0.361 0	0.285 6	0.639 6	97.55	99.02	1.08
	0.361 0	0.285 6	0.649 1	100.88
	0.361 0	0.285 6	0.646 4	99.93
	0.361 0	0.357 0	0.711 6	98.21
	0.361 0	0.357 0	0.710 8	97.98
	0.361 0	0.357 0	0.716 7	99.64
	0.361 0	0.428 4	0.783 1	98.53
	0.361 0	0.428 4	0.784 7	98.90
	0.361 0	0.428 4	0.787 6	99.58
绿原酸	5.929 0	4.715 2	10.593 3	98.92	98.21	1.1
	5.929 0	4.715 2	10.609 8	99.27
	5.929 0	4.715 2	10.612 0	99.32
	5.929 0	5.894 0	11.794 6	99.52
	5.929 0	5.894 0	11.701 5	97.94
	5.929 0	5.894 0	11.702 7	97.96
	5.929 0	7.072 8	12.785 9	96.95
	5.929 0	7.072 8	12.793 1	97.05
	5.929 0	7.072 8	12.784 3	96.92
咖啡酸	0.072 0	0.058 4	0.128 5	96.75	97.92	1.49
	0.072 0	0.058 4	0.130 1	99.49
	0.072 0	0.058 4	0.128 9	97.43
	0.072 0	0.073 0	0.142 3	96.30
	0.072 0	0.073 0	0.142 1	96.03
	0.072 0	0.073 0	0.144 9	99.86
	0.072 0	0.0876	0.159 1	99.43
	0.072 0	0.087 6	0.158 4	98.63
	0.072 0	0.087 6	0.157 3	97.37
木犀草苷	0.476 0	0.377 6	0.856 9	100.87	100.11	1.07
	0.476 0	0.377 6	0.843 7	97.38
	0.476 0	0.377 6	0.852 6	99.74
	0.476 0	0.472 0	0.949 4	100.30
	0.476 0	0.472 0	0.949 9	100.40
	0.476 0	0.472 0	0.950 8	100.59
	0.476 0	0.566 4	1.044 9	100.44
	0.476 0	0.566 4	1.046 5	100.72
	0.476 0	0.566 4	1.045 3	100.51
3,5-O-二咖啡酰基奎宁酸	1.216 0	0.967 2	2.168 1	98.44	98.22	1.27
	1.216 0	0.967 2	2.176 3	99.29
	1.216 0	0.967 2	2.160 9	97.69
	1.216 0	1.209 0	2.384 9	96.68
	1.216 0	1.209 0	2.381 3	96.39
	1.216 0	1.209 0	2.399 6	97.90
	1.216 0	1.450 8	2.671 4	100.32
	1.216 0	1.450 8	2.653 8	99.10
	1.216 0	1.450 8	2.640 5	98.19
4,5-O-二咖啡酰基奎宁酸	1.757 0	1.408 8	3.109 9	96.03	96.92	1.17
	1.757 0	1.408 8	3.110 7	96.09
	1.757 0	1.408 8	3.111 4	96.14
	1.757 0	1.761 0	3.469 1	97.22
	1.757 0	1.761 0	3.464 2	96.94
	1.757 0	1.761 0	3.450 6	96.17
	1.757 0	2.113 2	3.851 0	99.09
	1.757 0	2.113 2	3.836 5	98.41
	1.757 0	2.113 2	3.789 4	96.18
木犀草素	0.153 0	0.123 2	0.271 4	96.10	98.74	1.43
	0.153 0	0.123 2	0.274 9	98.94
	0.153 0	0.123 2	0.275 6	99.51
	0.153 0	0.154 0	0.306 3	99.55
	0.153 0	0.154 0	0.307 1	100.06
	0.153 0	0.154 0	0.306 4	99.61
	0.153 0	0.184 8	0.337 5	99.84
	0.153 0	0.184 8	0.334 6	98.27
	0.153 0	0.184 8	0.331 9	96.81
芹菜素	0.087 0	0.071 2	0.156 3	97.33	98.52	1.36
	0.087 0	0.071 2	0.157 9	99.58
	0.087 0	0.071 2	0.156 1	97.05
	0.087 0	0.089 0	0.174 2	97.98
	0.087 0	0.089 0	0.175 3	99.21
	0.087 0	0.089 0	0.173 0	96.63
	0.087 0	0.106 8	0.192 3	98.60
	0.087 0	0.106 8	0.193 7	99.91
	0.087 0	0.106 8	0.194 2	100.37
马钱苷	2.248 0	1.803 2	4.026 4	98.62	99.35	0.66
	2.248 0	1.803 2	4.031 5	98.91
	2.248 0	1.803 2	4.039 1	99.33
	2.248 0	2.254 0	4.516 7	100.65
	2.248 0	2.254 0	4.496 3	99.75
	2.248 0	2.254 0	4.495 6	99.72
	2.248 0	2.704 8	4.931 1	99.20
	2.248 0	2.704 8	4.912 0	98.49
	2.248 0	2.704 8	4.938 7	99.48
当药苷	0.687 0	0.553 6	1.229 4	97.98	98.97	1.22
	0.687 0	0.553 6	1.231 6	98.37
	0.687 0	0.553 6	1.224 7	97.13
	0.687 0	0.692 0	1.368 4	98.47
	0.687 0	0.692 0	1.379 3	100.04
	0.687 0	0.692 0	1.385 6	100.95
	0.687 0	0.830 4	1.517 1	99.96
	0.687 0	0.830 4	1.504 2	98.41
	0.687 0	0.830 4	1.512 7	99.43
断氧化马钱子苷	2.791 0	2.229 6	4.951 6	96.91	96.73	0.53
	2.791 0	2.229 6	4.954 3	97.03
	2.791 0	2.229 6	4.952 1	96.93
	2.791 0	2.787 0	5.470 9	96.16
	2.791 0	2.787 0	5.471 7	96.19
	2.791 0	2.787 0	5.469 1	96.09
	2.791 0	3.344 4	6.039 4	97.13
	2.791 0	3.344 4	6.019 2	96.53
	2.791 0	3.344 4	6.054 3	97.58
（R,S）-告依春	0.119 0	0.093 6	0.212 5	99.89	99.21	1.47
	0.119 0	0.093 6	0.210 4	97.65
	0.119 0	0.093 6	0.213 1	100.53
	0.119 0	0.117 0	0.235 3	99.40
	0.119 0	0.117 0	0.236 8	100.68
	0.119 0	0.117 0	0.235 7	99.74
	0.119 0	0.140 4	0.254 3	96.37
	0.119 0	0.140 4	0.257 1	98.36
	0.119 0	0.140 4	0.259 7	100.21
直铁线莲宁B	0.052 0	0.040 8	0.092 5	99.26	97.48	1.58
	0.052 0	0.040 8	0.091 4	96.57
	0.052 0	0.040 8	0.093 1	100.74
	0.052 0	0.051 0	0.101 3	96.67
	0.052 0	0.051 0	0.101 8	97.65
	0.052 0	0.051 0	0.101 1	96.27
	0.052 0	0.061 2	0.111 2	96.73
	0.052 0	0.061 2	0.110 9	96.24
	0.052 0	0.061 2	0.111 5	97.22

Tab. 2

Tab. 3

References 17

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组分	回归方程	r	线性范围/（μg/mL）
新绿原酸	Y=9.841 6×10⁵X-813.9	0.999 6	2.39~119.50
绿原酸	Y=1.351 2×10⁶X+1 543.1	0.999 2	40.65~2 032.50
咖啡酸	Y=5.982 4×10⁵X-1 813.6	0.999 3	0.49~24.50
木犀草苷	Y=1.523 9×10⁶X+613.8	0.999 1	3.06~153.00
3,5-O-二咖啡酰基奎宁酸	Y=6.931 8×10⁵X-961.4	0.999 9	7.95~397.50
4,5-O-二咖啡酰基奎宁酸	Y=1.109 7×10⁶X-846.2	0.999 4	11.88~594.00
木犀草素	Y=1.485 1×10⁶X-613.7	0.999 2	1.04~52.00
芹菜素	Y=8.330 6×10⁵X+516.5	0.999 3	0.56~28.00
马钱苷	Y=1.902 4×10⁶X-1 064.2	0.999 5	16.02~801.00
当药苷	Y=1.722 5×10⁶X-436.8	0.999 7	4.35~217.50
断氧化马钱子苷	Y=2.185 7×10⁶X+491.6	0.999 6	19.59~979.50
（R,S）-告依春	Y=1.215 9×10⁶X+1 162.3	0.999 8	0.77~38.50
直铁线莲宁B	Y=3.157 4×10⁵X-899.1	0.999 4	0.36~18.00

批号	含量/（mg/mL）
批号	新绿原酸	绿原酸	咖啡酸	木犀草苷	3,5-O-二咖啡酰基奎宁酸	4,5-O-二咖啡酰基奎宁酸	木犀草素	芹菜素	马钱苷	当药苷	断氧化马钱子苷	（R,S）-告依春	直铁线莲宁B
H2073	0.361	5.929	0.072	0.476	1.216	1.757	0.153	0.087	2.248	0.687	2.791	0.119	0.052
H2111	0.346	5.750	0.069	0.463	1.162	1.691	0.155	0.086	2.691	0.671	2.696	0.115	0.050
H2116	0.379	6.183	0.078	0.504	1.318	1.907	0.164	0.091	2.418	0.734	2.981	0.127	0.054

Determination of 13 chemical components in Koujie gargle by HPLC

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