高效液相色谱法测定洗发护发产品中18种防腐剂和去屑剂

doi:10.3969/j.issn.2097-2806.2024.04.014

Abstract

Abstract:

A high performance liquid chromatography （HPLC） method for simultaneous determination of 18 preservatives and anti-dandruff components in cosmetics of different bases was established, and the quality of 50 batches of commercially available shampoo and hair care cosmetics was analyzed. After the extraction of samples of different bases, the samples were analyzed by HPLC and quantified by external standard method. A C18 column （4.6 mm×250 mm, 5 μm） was used and an aqueous mixture of methanol and sodium dihydrogen phosphate （pH adjusted to 3.8） was selected as mobile phase for gradient elution. The flow rate was 1.0 mL/min. The column temperature was 30 ℃. The chromatographic separation of the 18 components was good. The linearity between peak area and mass concentration was good （r>0.998 3） in the range of 0.4-600 μg/mL, and the detection limit was 0.4-10 mg/kg. The average recoveries （n=6） were 83.1%-110.4%, the RSDs were 0.12%-7.6%, and the recoveries were good. These components remained stable within 24 h with RSDs ranging from 0.15% to 3.8%, indicative of good stability. Nine components were detected in 50 batches of samples, including pyrithione zinc, piroctone olamine, p-chloro-m-cresol, climbazole, triclosan and salicylic acid, whose content was 2 100-6 800, 39-2 900, 130-370, 24-1 600, 0.14-0.19, 28-1 900 mg/kg, respectively. Benzyl chlorophenol, o-aminophenol and o-cymen-5-ol were detected, but their content was less than the limit of quantitation and thus could not be accurately quantified. Therefore, this method could be used to simultaneously determine the 18 antiseptic and anti-dandruff components in cosmetics.

Key words: preservative, anti-dandruff agent, high performance liquid chromatography

CLC Number:

TQ658

Zhuangfei Zhu, Qinke Xu, Tingyuan Liu, Ying Sun, Hong Lei. Determination of 18 preservatives and anti-dandruff agents in shampoo and hair care products by HPLC[J].China Surfactant Detergent & Cosmetics, 2024, 54(4): 477-483.

Figures/Tables 4

Tab. 1

Fig. 1

Tab. 2

Tab. 3

Recoveries and RSDs of 18 components （n=6）"

组分名称	添加量/μg	回收率/%			RSD/%
组分名称	添加量/μg	粉基质	蜡基质	其他基质	粉基质	蜡基质	其他基质
ZiP	0.2	85.1	84.8	89.1	4.7	4.3	2.6
	2	89.3	86.2	95.7	3.6	2.6	1.9
	10	96.4	92.1	108.4	0.98	0.62	1.1
2，4-DiA	0.2	88.5	89.3	90.2	3.8	4.8	4.1
	2	95.2	95.8	98.5	1.7	3.8	2.6
	10	98.3	93.3	101.4	1.2	2.9	1.4
MeB	0.2	90.4	91.8	92.4	3.1	5.2	2.4
	2	95.6	95.3	95.3	1.9	4.1	1.2
	10	101.5	99.6	104.6	0.38	2.8	0.14
PeS	0.2	86.5	86.2	95.7	4.4	3.7	2.4
	2	95.7	88.3	94.8	2.4	3.4	0.87
	10	97.8	95.4	99.6	1.8	1.7	0.32
BeC	0.2	88.9	90.1	86.8	3.7	4.6	3.6
	2	90.6	92.3	96.3	1.7	3.7	1.9
	10	93.6	94.3	98.8	0.45	1.3	1.1
IbC	0.2	86.7	88.3	96.7	4.4	4.7	4.9
	2	95.8	94.7	93.8	4.1	3.6	3.7
	10	99.5	97.2	106.2	2.9	2.8	1.4
p-TcC	0.2	92.5	91.5	96.3	2.2	2.8	3.4
	2	98.6	98.5	93.2	1.5	2.2	1.6
	10	100.4	101.3	98.9	0.12	0.8	1.1
o-PhP	0.2	85.9	88.4	87.2	3.7	3.7	4.8
	2	94.9	95.3	92.2	1.4	2.8	4.1
	10	95.3	97.5	97.8	0.23	2.1	3.8
Or-5-O	0.2	87.5	89.5	86.7	3.6	4.4	2.5
	2	94.1	97.4	93.4	1.8	3.7	0.96
	10	98.6	95.1	98.6	1.5	3.1	0.55
ChX	0.2	87.8	90.3	92.5	3.2	4.7	2.6
	2	89.4	94.3	99.6	4.5	3.6	1.9
	10	95.1	92.1	100.7	3.7	0.98	1.1
ClB	0.2	88.5	86.3	90.6	7.2	3.8	4.1
	2	95	89.1	98.9	5.5	1.7	2.6
	10	98.4	91.7	99.6	3.5	1.2	1.4
TrC	0.2	92.8	94.3	95.3	4.4	3.1	2.4
	2	98.5	98.2	98.6	3.1	1.9	1.2
	10	103.5	101.2	96.4	1.4	0.38	0.14
TrS	0.2	95.6	89.8	94.6	3.3	4.4	2.4
	2	98	93.8	99.8	2.5	2.4	0.87
	10	98.6	106.2	110.4	0.8	1.8	0.32
SoA	0.2	86.3	93.9	90.6	3.6	3.7	3.6
	2	88.6	94.2	95.7	2.2	1.7	1.9
	10	93.4	98.7	91.8	1.5	0.45	1.1
SaA	0.2	85.3	86.2	96.7	6.2	4.4	4.9
	2	90.5	94.9	93.8	4.8	4.1	3.7
	10	96.7	103.2	104.7	2.1	2.9	1.4
BrF	0.2	88.5	87.3	94.6	4.2	2.2	3.4
	2	93.7	90.2	90.5	2.6	1.5	1.6
	10	95.8	96.8	98.8	1.1	0.12	1.1
PhA	0.2	84.8	83.1	85.3	7.6	6.2	4.8
	2	86.7	84.7	86.2	5.9	4.8	4.1
	10	91.7	88.4	90.5	4.6	3.9	3.8
2，6-DiA	0.2	92.8	89.4	87.9	4.8	5.2	2.5
	2	98.5	93.7	90.6	3.7	4.8	0.96
	10	97.8	95.8	98.4	1.6	3.6	0.55

Tab. 3

References 14

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序号	名称	英文缩写	纯度/%	批号	生产商
1	水杨酸	SaA	98.9	G146757	Dr.Ehrenstorfer公司
2	氯咪巴唑	ClB	99.4	G131864	Dr.Ehrenstorfer公司
3	山梨酸	SoA	99.18	G996530	Dr.Ehrenstorfer公司
4	苯氧异丙醇	PhA	99.8	G766231	Dr.Ehrenstorfer公司
5	对氯间甲酚	p-TcC	99.7	G168075	Dr.Ehrenstorfer公司
6	邻苯基苯酚	o-PhP	99	G451296	Dr.Ehrenstorfer公司
7	氯二甲酚	ChX	99.16	G1074553	Dr.Ehrenstorfer公司
8	苄氯酚	BeC	95.4	G1018113	Dr.Ehrenstorfer公司
9	三氯卡班	TrC	99	G161921	Dr.Ehrenstorfer公司
10	三氯生	TrS	99.9	G171100	Dr.Ehrenstorfer公司
11	溴氯芬	BrF	99.52	G1010500	Dr.Ehrenstorfer公司
12	吡硫鎓锌	ZiP	99.2	1217-RB-0018	Cato Resarch Chemicals Inc公司
13	吡罗克酮乙醇胺盐	PeS	94.3	1020-RB-0020	Cato Resarch Chemicals Inc公司
14	2，6-二氯苯甲醇	2，6-DiA	99.4	0312-RC-0027	Cato Resarch Chemicals Inc公司
15	碘丙炔醇丁基氨甲酸酯	IbC	98.6	0729-RB-0040	Cato Resarch Chemicals Inc公司
16	2，4-二氯苯甲醇	2，4-DiA	99.7	0315-RC-0023	Cato Resarch Chemicals Inc公司
17	邻伞花烃-5-醇	Or-5-O	99.7	0312-RC-0029	Cato Resarch Chemicals Inc公司
18	苯甲酸甲酯	MeB	97	1-LXM-88-1	TRC公司

组分名称	检测波长/nm	线性方程	R	线性范围/（μg/mL）	检出限/（mg/kg）	定量限/（mg/kg）
ZiP	280	Y=29.867 00X-66.233 49	0.999 8	0.4~40	10	33
2，4-DiA	230	Y=15.329 04X-25.179 18	0.999 7	2~200	4.0	13
MeB	230	Y=49.411 24X+20.717 79	0.998 3	0.6~60	1.0	3.3
PeS	230	Y=8.355 44X-17.555 09	0.999 3	2~200	4.0	13
BeC	230	Y=20.147 58X+9.682 67	0.998 5	0.6~60	1.0	3.3
IbC	230	Y=0.941 34X-5.551 40	0.999 5	6~600	10	33
p-TcC	230	Y=27.168 06X+11.895 84	0.998 4	0.6~60	1.0	3.3
o-PhP	230	Y=26.860 53X+12.842 60	0.998 5	0.6~60	1.0	3.3
Or-5-O	280	Y=5.903 64X+2.866 09	0.998 3	0.6~60	1.0	3.3
ChX	280	Y=5.475 42X-12.102 30	0.999 5	2~200	4.0	13
ClB	230	Y=13.824 46X-28.376 21	0.999 5	2~200	4.0	13
TrC	280	Y=29.170 38X+4.513 12	0.998 5	0.2~20	0.40	1.3
TrS	280	Y=9.176 35X+3.998 74	0.998 5	0.6~60	1.0	3.3
SoA	280	Y=53.697 87X+8.515 56	0.998 4	0.2~20	0.40	1.3
SaA	280	Y=6.956 37X+0.888 96	0.999 6	0.6~60	2.0	6.7
BrF	230	Y=21.565 52X+11.066 49	0.998 4	0.6~60	1.0	3.3
2，6-DiA	230	Y=6.465 14X-9.815 10	0.999 7	2~200	4.0	13
PhA	280	Y=1.921 07X+0.555 96	0.998 3	0.6~60	2.0	6.7

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Determination of 18 preservatives and anti-dandruff agents in shampoo and hair care products by HPLC

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