超高效液相色谱法快速测定化妆品中23种防腐剂

doi:10.3969/j.issn.1001-1803.2022.10.014

Abstract

Abstract:

A rapid analytical method for the simultaneous determination of 23 preservatives in cosmetics was established by ultra-high performance liquid chromatography （UPLC）. The sample was extracted with methanol and separated by CAPCELL CORE C₁₈ column （2.1 mm×150 mm, 2.7 μm） chromatographic column separation using 0.1% phosphoric acid acetonitrile as the mobile phase with gradient elution. The flow rate was 0.4 mL/min, and the detection wavelength was 280, 254 and 230 nm. The results show that the method has good methodological validation, good separation effect, short analysis time, simple operation and simple composition of mobile phase, which can be used for rapid detection of preservatives in daily cosmetics.

Key words: cosmetics, preservative, ultra performance liquid chromatography, rapid analysis

CLC Number:

TQ658

Zhang Weiqing,Liu Huijin,Wang Haiyan,Sun Lei. Rapid determination of 23 preservatives in cosmetics by ultra performance liquid chromatography[J].China Surfactant Detergent & Cosmetics, 2022, 52(10): 1128-1134.

Figures/Tables 6

Tab. 1

Tab. 2

Fig. 1

Tab. 3

Tab. 4

Recovery and precision of 23 preservatives"

组分	添加量/（μg/mL）	膏霜		油基		香波
组分	添加量/（μg/mL）	回收率/%	RSD/%	回收率/%	RSD/%	回收率/%	RSD/%
甲基异噻唑啉酮	0.1	108.3	3.93	106.4	4.52	110.2	3.94
	0.2	119.4	3.25	110.9	4.76	113.3	4.02
	0.4	110.9	4.16	107.7	4.32	109.7	3.83
2-溴-2硝基丙烷-1,3二醇	3.75	107.5	2.13	103.5	2.54	111.9	3.23
	7.5	110.9	2.52	111.5	4.26	109.9	3.30
	15	114.7	4.95	107.6	4.28	102.0	4.20
4-羟基苯甲酸	0.5	117.6	3.01	112.3	4.27	112.4	3.43
	1	117.4	2.35	113.1	3.97	113.5	2.83
	2	113.5	3.59	108.5	3.72	111.7	2.72
甲基氯异噻唑啉酮	0.1	114.4	2.41	104.3	3.73	101.8	3.69
	0.2	107.5	2.96	106.9	4.05	107.4	3.70
	0.4	110.2	1.86	106.0	2.35	109.5	3.64
苯甲醇	7.5	113.3	2.33	110.4	3.63	119.9	3.71
	15	113.2	3.25	109.5	2.48	109.7	2.35
	30	110.3	1.29	106.8	2.33	110.0	3.05
苯氧乙醇	5	115.3	1.96	112.0	1.97	114.5	2.38
	10	115.3	2.45	110.9	3.43	110.1	2.05
	20	110.1	2.33	106.6	1.21	108.8	2.13
苯甲酸	1.25	112.1	3.17	104.0	4.05	107.1	3.13
	2.5	115.7	2.84	107.3	3.96	107.5	2.99
	5	111.4	2.73	107.2	3.75	110.2	3.70
4-羟基苯甲酸甲酯	0.312 5	88.2	3.89	85.7	4.45	87.1	3.49
	0.625	105.8	4.30	99.4	3.26	104.0	3.05
	1.25	121.2	3.47	100.8	3.08	111.2	2.30
氯苯甘醚	0.75	101.6	2.82	92.4	3.06	99.7	3.30
	1.5	109.2	1.96	105.9	2.98	105.3	2.24
	3	104.0	1.88	102.2	2.64	104.6	3.20
脱氢乙酸	0.75	101.4	1.98	105.3	2.99	105.1	2.34
	1.5	109.5	1.75	106.4	3.35	106.6	4.01
	3	105.5	3.06	102.2	4.53	104.3	4.35
5-溴-5-硝基-1,3-二噁烷	6.25	114.7	2.99	110.9	3.28	113.5	4.35
	12.5	115.1	3.53	111.0	3.43	110.8	3.95
	25	111.0	3.61	106.3	3.62	109.3	3.78
4-羟基苯甲酸乙酯	0.625	110.8	2.82	107.0	3.48	108.7	2.67
	1.25	105.0	2.05	101.0	3.23	100.8	3.06
	2.5	108.0	3.40	103.7	3.61	103.9	3.83
4-羟基苯甲酸异丙酯	0.625	110.6	2.68	107.1	3.85	107.3	4.06
	1.25	114.9	4.02	107.2	4.24	108.2	4.13
	2.5	108.4	3.64	103.7	3.98	106.3	3.25
4-羟基苯甲酸丙酯	0.625	104.6	4.05	96.7	4.67	108.1	4.06
	1.25	104.1	3.88	110.9	4.36	99.2	3.97
	2.5	113.9	4.42	93.5	4.25	108.5	4.28
4-羟基苯甲酸苯酯	0.75	113.8	3.75	110.6	3.68	110.1	3.12
	1.5	113.9	2.99	109.3	2.98	110.2	3.20
	3	109.1	3.74	104.1	2.74	106.9	3.23
4-羟基苯甲酸异丁酯	0.75	110.0	2.99	104.9	3.15	105.3	3.24
	1.5	111.2	3.62	106.6	2.98	106.9	3.75
	3	107.4	3.73	102.2	2.77	105.1	2.98
4-羟基苯甲酸丁酯	0.75	119.6	4.32	114.6	2.94	115.6	3.63
	1.5	116.6	4.05	112.2	4.00	114.0	3.58
	3	109.1	4.58	103.4	3.68	105.9	4.54
4-羟基苯甲酸苄酯	0.75	98.4	2.01	89.7	3.74	85.7	3.76
	1.5	92.6	3.60	88.6	2.86	90.7	2.82
	3	89.8	2.66	89.9	1.45	90.2	4.76
苯甲酸乙酯	1.5	109.8	2.23	104.9	2.76	104.7	4.05
	3	110.5	2.81	105.8	3.10	105.9	4.10
	6	106.1	3.81	101.7	2.83	104.2	4.28
4-羟基苯甲酸戊酯	1.5	109.0	2.05	105.5	2.24	104.1	2.75
	3	110.2	3.62	105.0	3.33	105.7	2.86
	6	105.4	3.83	100.1	4.05	103.4	3.64
苯甲酸异丙酯	1.75	100.0	3.75	97.4	2.98	94.9	3.45
	3.5	102.5	2.20	96.9	2.67	97.1	3.05
	7	95.9	1.24	92.2	2.34	96.2	2.56
苯甲酸丙酯	1.75	94.2	1.53	93.3	3.87	87.3	2.93
	3.5	100.6	2.05	93.7	2.75	94.8	2.73
	7	93.9	1.60	91.0	2.07	94.0	2.35
苯甲酸苯基酯	2	91.6	4.30	90.2	3.43	93.7	4.05
	4	119.7	2.98	110.5	4.12	114.8	3.68
	8	105.5	3.99	96.3	4.05	103.6	3.49

Tab. 4

Tab. 5

References 17

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组分	线性方程	R²	线性范围/ （mg/L）	检出限/ng	定量限/ng
甲基异噻唑啉酮	y=16 415.6x+51.3	0.999 9	0.04~4.00	3	9
2-溴-2硝基丙烷-1,3二醇	y=74.6x-15.76	0.999 9	1.50~750.00	346	1 154
4-羟基苯甲酸	y=8 082.7x-579.0	0.999 9	0.20~100.00	6	19
甲基氯异噻唑啉酮	y=11 519.0x-206.5	0.999 9	0.04~20.00	4	13
苯甲醇	y=411.8x-442.9	0.999 9	3.00~1 500.00	120	400
苯氧乙醇	y=1 103.4x+2 384.7	0.999 9	2.00~1 000.00	48	158
苯甲酸	y=1 751.1x-999.4	0.999 9	0.50~250.00	34	112
4-羟基苯甲酸甲酯	y=8 599.5x-335.2	0.999 9	0.12~62.50	7	24
氯苯甘醚	y=790.0x+331.9	0.999 8	0.30~150.00	88	293
脱氢乙酸	y=6 667.3x-1 791.9	0.999 9	0.30~150.00	10	33
5-溴-5-硝基-1,3-二噁烷	y=262.4x-255.8	0.999 9	2.50~1 250.00	224	746
4-羟基苯甲酸乙酯	y=7 877.6x+2.9	0.999 9	0.25~125.00	8	27
4-羟基苯甲酸异丙酯	y=6 257.5x+87.4	0.999 9	0.25~125.00	9	31
4-羟基苯甲酸丙酯	y=5 564.2x-122.1	0.999 9	0.25~125.00	10	34
4-羟基苯甲酸苯酯	y=13 137.0x-815.3	0.999 9	0.30~150.00	6	18
4-羟基苯甲酸异丁酯	y=5 864.2x-279.9	0.999 9	0.30~150.00	13	43
4-羟基苯甲酸丁酯	y=4 808.8x-344.3	0.999 9	0.30~150.00	16	53
4-羟基苯甲酸苄酯	y=2 058.2x-1 055.2	0.999 9	0.30~150.00	46	153
苯甲酸乙酯	y=3 237.2x-1 022.2	0.999 9	0.60~300.00	27	90
4-羟基苯甲酸戊酯	y=5 019.1x-677.3	0.999 8	0.60~300.00	19	63
苯甲酸异丙酯	y=1 006.8x-1 566.5	0.999 8	0.70~350.00	113	377
苯甲酸丙酯	y=1 141.1x-1 633.5	0.999 9	0.70~350.00	89	297
苯甲酸苯基酯	y=1 680.0x+3 610.4	0.999 6	0.80~400.00	35	115

样品/组分	检测结果/（μg/g）
样品/组分	**牌沐浴露	**牌泡泡沐浴露	**牌护臀膏	**牌维E面霜	**牌维E润肤乳	**牌护肤油	**牌止痒膏
苯氧乙醇	nd	nd	3 721.83	4 013.30	2 308.97	2 004.83	nd
4-羟基苯甲酸甲酯	nd	nd	nd	845.42	1 382.96	1 023.74	nd
4-羟基苯甲酸乙酯	nd	nd	nd	nd	364.98	317.44	nd

Rapid determination of 23 preservatives in cosmetics by ultra performance liquid chromatography

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名称	混合标准系列溶液质量浓度/（μg/mL）
名称	1	2	3^*	4	5	6
甲基异噻唑啉酮	20	4	2	0.4	0.2	0.1
2-溴-2硝基丙烷-1, 3二醇	750	150	75	15	7.5	3.75
4-羟基苯甲酸	100	20	10	2	1	0.5
甲基氯异噻唑啉酮	20	4	2	0.4	0.2	0.1
苯甲醇	1 500	300	150	30	15	7.5
苯氧乙醇	1 000	200	100	20	10	5
苯甲酸	250	50	25	5	2.5	1.25
4-羟基苯甲酸甲酯	62.5	12.5	6.25	1.25	0.625	0.312 5
氯苯甘醚	150	30	15	3	1.5	0.75
脱氢乙酸	150	30	15	3	1.5	0.75
5-溴-5-硝基-1, 3-二噁烷	1 250	250	125	25	12.5	6.25
4-羟基苯甲酸乙酯	125	25	12.5	2.5	1.25	0.625
4-羟基苯甲酸异丙酯	125	25	12.5	2.5	1.25	0.625
4-羟基苯甲酸丙酯	125	25	12.5	2.5	1.25	0.625
4-羟基苯甲酸苯酯	150	30	15	3	1.5	0.75
4-羟基苯甲酸异丁酯	150	30	15	3	1.5	0.75
4-羟基苯甲酸丁酯	150	30	15	3	1.5	0.75
4-羟基苯甲酸苄酯	150	30	15	3	1.5	0.75
苯甲酸乙酯	300	60	30	6	3	1.5
4-羟基苯甲酸戊酯	300	60	30	6	3	1.5
苯甲酸异丙酯	350	70	35	7	3.5	1.75
苯甲酸丙酯	350	70	35	7	3.5	1.75
苯甲酸苯基酯	400	80	40	8	4	2

t/min	φ（A）/%	φ（B）/%	t/min	φ（A）/%	φ（B）/%
0	95	5	18	35	65
1	95	5	19	10	90
1.1	85	15	22	10	90
8	70	30	22.1	95	5
10	60	40	25	95	5
15	60	40

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