超高效液相色谱-串联质谱法测定化妆品中乳糖酸等8种有机酸

doi:10.3969/j.issn.2097-2806.2023.08.016

Abstract

Abstract:

The study aims to establish a method for the determination of eight organic acids in cosmetics, including lactobionic acid, L-lactic acid, citric acid, succinic acid, DL-mandelic acid, ferulic acid, azelaic acid and lipoic acid, by ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）. The chromatographic column was Waters ACQUITY UPLC^® HSS T3 column （1.8 μm, 2.1 mm×100 mm） with methanol-water （volume ratio 50∶50） as the extraction solution and ammonium acetate （pH=2.6） -water-acetonitrile as the mobile phases. The flow rate is 0.35 mL/min and the column temperature is 35 ℃. The electrospray ion （ESI） source, negative ions scanning method and multiple reaction monitoring （MRM） mode are used to determine the content. There are good linear relationships （R²≥0.99） and the peak area of the eight organic acids are 2.52-10.10, 4.54-18.16, 2.82-15.30, 2.30-9.22, 2.41-9.63, 2.27-9.08, 2.33-9.33, and 2.16-8.65 μg/mL, respectively. Their minimum limits of quantitation （LOQ） are as low as 0.003 μg/g. The RSDs of precision, stability and repeatability tests are all less than 7.79%. The recoveries of high, medium and low concentrations range from 86.52% to 119.98%, with RSD ranging from 0.55% to 4.74%. The method has high accuracy, good repeatability and fast speed, and is suitable for the simultaneous determination of eight organic acids in cosmetics.

Key words: UPLC-MS/MS, cosmetics

CLC Number:

TQ658

Zhang Xin,Huo Yongli. Determination of eight organic acids such as lactobionic acid in cosmetics by ultra performance liquid chromatography-tandem mass spectrometry[J].China Surfactant Detergent & Cosmetics, 2023, 53(8): 981-988.

Figures/Tables 10

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References 20

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序号	中文名称	CAS NO.	化学式	分子量
1	乳糖酸	96-82-2	C₁₂H₂₂O₁₂	358.11
2	L-乳酸	79-33-4	C₃H₆O₃	90.03
3	柠檬酸	77-92-9	C₆H₈O₇	192.12
4	琥珀酸	110-15-6	C₄H₆O₄	118.09
5	DL-扁桃酸	90-64-2	C₈H₈O₃	152.15
6	阿魏酸	1135-24-6	C₁₀H₁₀O₄	194.18
7	壬二酸	123-99-9	C₉H₁₆O₄	188.22
8	硫辛酸	62-46-4	C₈H₁₄O₂S₂	206.32

物质名称	保留时间/min	母离子/（m/z）	定量子离子/（m/z）	锥孔电压/V	碰撞电压/V
乳糖酸	0.74	357.14	74.86	-60	-24
L-乳酸	1.13	89.02	42.85	-10	-8
柠檬酸	1.14	191.02	110.80	-5	-10
琥珀酸	1.58	117.02	72.90	-10	-10
DL-扁桃酸	3.18	151.04	106.85	-10	-7
阿魏酸	3.68	193.06	133.95	-20	-13
壬二酸	3.81	187.10	125.00	-10	-13
硫辛酸	4.31	205.04	171.02	-10	-7

序号	物质名称	回归方程	相关系数R²	线性范围/ （μg/mL）	检出限/（μg/g）		定量限/（μg/g）
序号	物质名称	回归方程	相关系数R²	线性范围/ （μg/mL）	标样	基质	标样	基质
1	乳糖酸	y=5 384.8x-4.858 4	0.998 9	2.52~10.10	0.058 5	0.059 8	0.195 1	0.199 4
2	L-乳酸	y=3 118.1x+3 366.5	0.994 4	4.54~18.16	0.110 8	0.115 6	0.369 2	0.385 3
3	柠檬酸	y=45 699x-91 179	0.993 5	2.82~15.30	0.821 3	0.752 3	2.737 7	2.507 7
4	琥珀酸	y=30 536x+1 899.5	0.996 9	2.30~9.22	0.617 6	0.431 7	2.058 7	1.439 1
5	DL-扁桃酸	y=24 484x-9 502.8	0.996 4	2.41~9.63	0.039 8	0.038 3	0.132 6	0.127 8
6	阿魏酸	y=39 069x+4 515.4	0.997 6	2.27~9.08	0.003 0	0.003 0	0.009 8	0.009 8
7	壬二酸	y=60 951x+27 716	0.993 3	2.33~9.33	0.008 4	0.011 0	0.028 1	0.036 5
8	硫辛酸	y=31 606x+8 818.3	0.992 9	2.16~8.65	0.007 4	0.014 0	0.024 5	0.046 6

物质名称	质量浓度/ （μg/mL）	峰面积						平均值	RSD/%
乳糖酸	4.04	23 335	23 269	23 960	23 751	24 135	23 281	23 621.83	1.60
乳糖酸	10.10	56 223	55 836	55 136	53 670	54 657	53 375	54 816.17	2.09
L-乳酸	7.26	25 250	25 422	25 404	25 853	26 325	25 139	25 565.50	1.74
L-乳酸	18.16	58 472	57 646	54 905	57 010	55 151	58 951	57 022.50	2.95
柠檬酸	6.12	212 538	217 170	223 617	237 299	232 067	218 991	223 613.67	4.22
柠檬酸	15.30	620 061	611 290	619 066	586 854	615 125	606 304	609 783.33	2.02
琥珀酸	3.71	117 104	117 650	121 515	121 119	121 864	119 485	119 789.50	1.71
琥珀酸	9.26	284 346	287 989	280 902	281 478	275 181	277 416	281 218.67	1.64
DL-扁桃酸	3.89	82 679	84 015	86 676	88 699	87 879	85 188	85 856.00	2.70
DL-扁桃酸	9.73	224 699	225 558	225 922	222 531	218 985	222 878	223 428.83	1.15
阿魏酸	3.64	160 888	158 365	157 648	160 856	163 224	157 631	159 768.67	1.41
阿魏酸	9.11	378 154	374 072	375 576	376 649	373 125	369 739	374 552.50	0.79
壬二酸	3.77	287 926	283 524	280 223	288 268	299 152	290 992	288 347.50	2.26
壬二酸	9.42	653 660	651 432	637 448	645 377	647 311	643 942	646 528.33	0.89
硫辛酸	3.52	135 627	135 351	135 004	132 607	124 936	136 863	133 398.00	3.28
硫辛酸	8.79	302 356	308 517	310 340	316 360	300 700	315 477	308 958.33	2.10

物质名称	质量浓度/（μg/mL）	峰面积			平均值	RSD/%
乳糖酸	4.04	23 622	21 947	22 419	22 662	3.81
乳糖酸	10.10	54 816	48 748	47 483	50 349	7.79
L-乳酸	7.26	25 566	26 482	27 956	26 668	4.52
L-乳酸	18.16	57 023	57 371	53 265	55 886	4.07
柠檬酸	6.12	223 614	196 600	211 461	210 558	6.43
柠檬酸	15.30	609 783	596 426	618 120	608 110	1.80
琥珀酸	3.71	119 790	121 519	129 068	123 459	4.00
琥珀酸	9.26	281 219	294 584	308 674	294 826	4.66
DL-扁桃酸	3.89	85 856	84 187	91 294	87 112	4.27
DL-扁桃酸	9.73	223 429	217 739	234 690	225 286	3.83
阿魏酸	3.64	159 769	161 737	172 633	164 713	4.21
阿魏酸	9.11	374 553	380 324	400 487	385 121	3.54
壬二酸	3.77	288 348	292 393	302 310	294 350	2.44
壬二酸	9.42	646 528	649 198	668 620	654 782	1.84
硫辛酸	3.52	133 398	134 397	141 342	136 379	3.17
硫辛酸	8.79	308 958	306 267	316 565	310 597	1.72

Determination of eight organic acids such as lactobionic acid in cosmetics by ultra performance liquid chromatography-tandem mass spectrometry

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时间/min	流速/ （mL/min）	φ（A）/%	φ（B）/%	φ（C）/%
0.0	0.35	15	83	2
0.5	0.35	15	83	2
1.5	0.35	15	55	30
2.0	0.35	15	55	30
3.0	0.35	15	0	85
5.0	0.35	15	0	85
5.1	0.35	15	83	2
7.5	0.35	15	83	2

序号	物质名称	回收率/%			RSD/%
序号	物质名称	10 μg/mL	4 μg/mL	0.5 μg/mL	10 μg/mL	4 μg/mL	0.5 μg/mL
1	乳糖酸	105.97	89.95	86.52	0.70	0.55	1.75
2	L-乳酸	105.69	103.23	109.89	2.43	1.90	2.16
3	柠檬酸	105.06	96.28	119.98	2.98	3.14	4.74
4	琥珀酸	103.92	101.52	96.46	1.36	1.39	2.06
5	DL-扁桃酸	104.54	100.06	101.69	1.39	1.36	0.64
6	阿魏酸	105.45	100.31	97.79	0.80	0.82	2.18
7	壬二酸	105.95	99.44	96.07	1.49	3.13	3.30
8	硫辛酸	101.97	102.41	97.28	1.62	1.89	3.46

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