高效液相色谱-串联质谱法快速测定护肤透明质酸中抗菌药物

doi:10.3969/j.issn.1001-1803.2022.06.015

摘要/Abstract

摘要：

建立护肤透明质酸中抗生素类和硝基咪唑类两大类抗菌药物的高效液相色谱-串联质谱快速测定方法。分别选取两类抗菌药物各10种试剂,通过涡旋振荡、超声提取以及离心处理和过滤后,制备了两类抗菌药物的混合溶液。经色谱柱分离,梯度洗脱下通过正离子模式电喷雾电离,多反应监测模式检测。测定结果表明：两种抗菌药物的溶液样本中,各自含有的10种化合物成分的总离子均在不同时间下发生分离,并产生相应的响应值,呈现较好的线性关联,相关系数分别在0.997和0.996以上。两种抗菌药物的检出限、定量限分别为1.6,6 mg/kg和0.9~201,5~401 mg/kg。该方法准确、高效,适用于护肤透明质酸中抗生素类和硝基咪唑类抗菌药物的快速测定。

关键词: 高效液相色谱-串联质谱, 快速测定, 护肤透明质酸, 抗菌药物

Abstract:

The aim was to establish a rapid method for the determination of antibiotics and nitroimidazoles in skin care hyaluronic acid by high performance liquid chromatography tandem mass spectrometry. Ten reagents for each of the two kinds of antibiotics were selected. After vortex oscillation, ultrasonic extraction, centrifugation and filtration, the mixed solution samples of the two kinds of antibiotics were prepared. They were separated by chromatographic column, ionized by electrospray ionization in positive ion mode and detected by multiple reaction monitoring mode under gradient elution. The results show that the total ions of 10 compounds contained in the solution samples of the two antibiotics have separation reactions at different times and produce corresponding response values, showing a good linear correlation. The correlation coefficient results are 0.997 and above 0.996, respectively. The detection limits and quantitative limits of the two antibiotics are 1.6, 6 mg/kg, 0.9-201 mg/kg and 5-401 mg/kg, respectively. The method can accurately and efficiently complete the rapid determination of antibiotics and nitroimidazoles in skin care hyaluronic acid.

Key words: high performance liquid chromatography-tandem mass spectrometry, rapid determination, skin care hyaluronic acid, antibacterial drugs

中图分类号:

TQ658

张君芳. 高效液相色谱-串联质谱法快速测定护肤透明质酸中抗菌药物[J]. 日用化学工业, 2022, 52(6): 677-682.

Zhang Junfang. Rapid determination of antibacterial agents in skin care hyaluronic acid by high performance liquid chromatography-tandem mass spectrometry[J]. China Surfactant Detergent & Cosmetics, 2022, 52(6): 677-682.

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参考文献 15

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时间/min	φ（A）/%	φ（B）/%
0	80	20
30	70	30
50	30	70
51	80	20
55	80	20

化合物成分	保留时间/min	母离子（m/z）	子离子（m/z）	裂解电压/V	碰撞电压/V
恩诺沙星	4.17	321.1	303.1	55	32
恩诺沙星	4.17	321.1	232.1	55	27
环丙沙星	4.76	332.4	288.2	85	31
环丙沙星	4.76	332.4	245.1	85	26
诺氟沙星	4.56	320.2	276.1	55	26
诺氟沙星	4.56	320.2	233.2	55	36
氧氟沙星	4.57	362.4	318.3	70	28
氧氟沙星	4.57	362.4	261.1	70	38
双氟沙星	6.33	400.4	356.3	85	35
双氟沙星	6.33	400.4	299.2	85	29
司帕沙星	6.32	393.6	349.3	70	30
司帕沙星	6.32	393.6	292.3	70	36
加替沙星	4.36	376.4	332.4	60	25
加替沙星	4.36	376.4	281.2	60	37
丹诺沙星	4.94	358.2	340.3	55	28
丹诺沙星	4.94	358.2	283.3	55	35
氟罗沙星	4.57	362.4	318.3	80	28
氟罗沙星	4.57	362.4	261.1	80	39
麻保沙星	4.25	363.2	320.3	60	24
麻保沙星	4.25	363.2	345.3	60	30

化合物成分	保留时间/min	母离子（m/z）	子离子（m/z）	裂解电压/V	碰撞电压/V
4-硝基咪唑	3.21	114.3	68.3	30	16
4-硝基咪唑	3.21	114.3	84.1	30	13
羟基甲硝唑	4.47	188.3	123.3	25	16
羟基甲硝唑	4.47	188.3	126.3	25	15
羟基异丙硝唑	10.61	186.3	168.3	25	16
羟基异丙硝唑	10.61	186.3	122.3	25	21
异丙硝唑	13.23	170.3	124.3	35	18
异丙硝唑	13.23	170.3	109.3	35	25
甲硝唑	5.51	172.3	128.3	25	16
甲硝唑	5.51	172.3	82.2	25	21
奥硝唑	11.07	220.3	128.3	30	16
奥硝唑	11.07	220.3	82.2	30	26
洛硝哒唑	6.92	201.3	140.3	20	13
洛硝哒唑	6.92	201.3	55.3	20	21
替硝唑	9.39	248.3	121.3	30	16
替硝唑	9.39	248.3	128.3	30	21
苯硝咪唑	7..66	164.3	118.3	35	19
苯硝咪唑	7..66	164.3	91.2	35	31
氯甲硝咪唑	8.93	162.3	116.2	30	18
氯甲硝咪唑	8.93	162.3	145.2	30	16

化合物成分	相关系数	检出限/ （mg/kg）	定量限/ （mg/kg）
恩诺沙星	0.999 2	1.6	6
环丙沙星	0.999 8
诺氟沙星	0.999 8
氧氟沙星	0.999 7
双氟沙星	0.999 8
司帕沙星	0.999 7
加替沙星	0.999 4
丹诺沙星	0.999 6
氟罗沙星	0.999 4
麻保沙星	0.997 2

化合物成分	相关系数	检出限/ （mg/kg）	定量限/ （mg/kg）
4-硝基咪唑	0.999 6	41	201
羟基甲硝唑	0.999 7	5	21
羟基异丙硝唑	0.998 9	201	401
异丙硝唑	0.998 6	0.9	5
甲硝唑	0.999 5	9	21
奥硝唑	0.998 4	3	5
替硝唑	0.998 8	0.9	5
苯硝咪唑	0.999 1	9	21
洛硝哒唑	0.996 4	9	21
氯甲硝咪唑	0.998 7	21	41