气相色谱-质谱联用法测定婴幼儿化妆品中18种防腐剂

doi:10.3969/j.issn.1001-1803.2023.03.014

Abstract

Abstract:

A gas chromatography-mass spectrometry （GC-MS） method was established for the determination of 18 preservatives compounds （methyl chloride isothiazolinone, etc.） in infant cosmetics. The cosmetic samples were extracted with 0.1 mg/mL ascorbic acid methanol as the solvent, separated on an Agilent DB-5 MS chromatographic column （30 m×0.25 mm×0.25 μm） by temperature programming with split injection technique, analyzed by GC-MS, and then quantified by an external standard curve. The results indicate that the effective separation and determination of 18 preservatives can be realized within 20 minutes. The method has good linear relationship with the correlation coefficients （R） greater than 0.998, the limits of detection （LOD） are in the ranges of 0.15-1.50 μg/kg, and the average recoveries at three spiked levels are in the range of 76.7%-104.9%. The method is accurate, rapid, simple, and quite suitable for the simultaneous determination of 18 preservatives in infant cosmetics.

Key words: gas chromatography-mass spectrometry, infant cosmetics, preservative

CLC Number:

TQ658

Li Yuli, Xiao Ruina, Li Yanan, Tang Qikui, Wang Qilin, Han Xiaoping. Determination of 18 preservatives in infant cosmetics by gas chromatography-mass spectrometry[J].China Surfactant Detergent & Cosmetics, 2023, 53(3): 349-354.

Figures/Tables 6

Tab. 1

Fig. 1

Fig. 2

Tab. 2

Tab. 3

Tab. 4

References 10

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序号	保留时间/min	名称	定量离子/ （m/z）	定性离子1/ （m/z）	定性离子2/ （m/z）	定性离子3/ （m/z）
1	5.4	甲基氯异噻唑啉酮	149	57	85	/
2	4.8	甲基异噻唑啉酮	115	87	58	/
3	3.2	苯甲醇	108	79	107	/
4	5.3	苯氧乙醇	138	94	77	/
5	4.7	苯甲酸	105	122	77	/
6	8.2	4-羟基苯甲酸甲酯	121	152	93	/
7	9.0	4-羟基苯甲酸乙酯	121	166	138	/
8	9.4	4-羟基苯甲酸异丙酯	121	138	180	/
9	10.2	4-羟基苯甲酸丙酯	121	138	180	/
10	11.1	4-羟基苯甲酸异丁酯	121	138	65	/
11	11.7	4-羟基苯甲酸丁酯	121	138	194	/
12	3.6	山梨酸	97	112	67	/
13	7.1	脱氢乙酸	168	153	125	/
14	5.6	苯氧异丙醇	94	152	65	66
15	11.6	氯苯甘醚	128	65	100	202
16	8.8	十二烷基二甲基苄基氯化铵	212	213	214	/
17	11.4	十四烷基二甲基苄基氯化铵	240	241	242	/
18	14.6	十六烷基二甲基苄基氯化铵	268	269	270	/

序号	名称	回归方程	R	检出限/（μg/kg）	定量限/（μg/kg）
1	甲基氯异噻唑啉酮	y=128 200x-253 400	0.998	0.30	0.85
2	甲基异噻唑啉酮	y=145 700x-637 800	0.998	0.25	0.75
3	苯甲醇	y=182 800x-478 500	0.998	0.50	1.50
4	苯氧乙醇	y=256 500x-736 900	0.998	0.50	1.50
5	苯甲酸	y=185 800x-908 000	0.998	0.60	2.00
6	4-羟基苯甲酸甲酯	y =342 900x-455 800	0.998	0.15	0.50
7	4-羟基苯甲酸乙酯	y=366 000x-483 300	0.998	0.15	0.50
8	4-羟基苯甲酸异丙酯	y=342 000x-399 400	0.999	0.30	1.20
9	4-羟基苯甲酸丙酯	y=275 100x-548 200	0.998	0.35	1.25
10	4-羟基苯甲酸异丁酯	y=347 600x-705 900	0.998	0.30	1.20
11	4-羟基苯甲酸丁酯	y=325 800x-715 000	0.998	0.30	1.20
12	山梨酸	y=103 400x-1 802 000	0.998	1.50	4.50
13	脱氢乙酸	y=121 600x-393 900	0.998	0.65	1.95
14	苯氧异丙醇	y=343 500x-585 000	0.998	0.55	1.65
15	氯苯甘醚	y=142 600x-1 779 000	0.998	1.25	3.75
16	十二烷基二甲基苄基氯化铵	y=7 365x-10 040	0.999	0.90	2.75
17	十四烷基二甲基苄基氯化铵	y=5 146x+4 208	0.999	0.90	2.75
18	十六烷基二甲基苄基氯化铵	y=3 296x+2 582	0.999	0.90	2.75

序号	名称	平均回收率/%			RSD/%
序号	名称	低	中	高	低	中	高
1	甲基氯异噻唑啉酮	83.2	85.3	85.5	3.2	2.6	2.4
2	甲基异噻唑啉酮	84.3	86.4	96.2	2.9	1.6	2.5
3	苯甲醇	85.9	90.6	101.1	3.4	2.9	2.8
4	苯氧乙醇	92.5	98.2	100.9	3.3	3.0	3.1
5	苯甲酸	93.0	96.9	102.3	6.3	5.5	5.0
6	4-羟基苯甲酸甲酯	95.6	101.2	98.4	4.2	3.6	4.0
7	4-羟基苯甲酸乙酯	94.9	99.6	102.7	2.9	2.7	3.1
8	4-羟基苯甲酸异丙酯	96.3	102.8	99.2	3.6	3.3	3.3
9	4-羟基苯甲酸丙酯	99.2	104.9	98.7	3.1	3.2	3.5
10	4-羟基苯甲酸异丁酯	95.9	97.8	100.0	3.8	3.4	3.2
11	4-羟基苯甲酸丁酯	94.2	98.5	100.7	3.7	3.1	2.7
12	山梨酸	76.7	89.2	90.6	4.0	3.7	2.9
13	脱氢乙酸	83.8	95.7	97.5	3.1	3.2	2.8
14	苯氧异丙醇	88.0	94.8	91.8	3.5	2.9	4.0
15	氯苯甘醚	89.1	104.3	95.4	3.9	3.8	4.5
16	十二烷基二甲基苄基氯化铵	85.7	92.4	93.0	5.0	4.8	4.5
17	十四烷基二甲基苄基氯化铵	84.9	86.9	90.8	5.1	4.6	6.2
18	十六烷基二甲基苄基氯化铵	82.9	85.3	88.4	5.2	5.7	6.4

序号	名称	检出批次	使用频率/%
1	甲基氯异噻唑啉酮	/	/
2	甲基异噻唑啉酮	15	30
3	苯甲醇	7	14
4	苯氧乙醇	33	66
5	苯甲酸	23	46
6	4-羟基苯甲酸甲酯	15	30
7	4-羟基苯甲酸乙酯	/	/
8	4-羟基苯甲酸异丙酯	/	/
9	4-羟基苯甲酸丙酯	12	24
10	4-羟基苯甲酸异丁酯	/	/
11	4-羟基苯甲酸丁酯	/	/
12	山梨酸	19	38
13	脱氢乙酸	21	42
14	苯氧异丙醇	/	/
15	氯苯甘醚	1	2
16	十二烷基二甲基苄基氯化铵	/	/
17	十四烷基二甲基苄基氯化铵	/	/
18	十六烷基二甲基苄基氯化铵	/	/

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Determination of 18 preservatives in infant cosmetics by gas chromatography-mass spectrometry

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