[Determination of 22 organic ultraviolet absorbers in human serum by ultra performance liquid chromatography- tandem mass spectrometry].

De-Jun Bao, Zhuang-Zhuang Feng, Xu Zhang, Qi Sun, Zhuo-Na Zhang, Xiao-Jian Hu, Ying Zhu, Xiao Lin
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Abstract

In this study, a method for the simultaneous determination of 22 organic ultraviolet absorbers (OUVs) in human serum was established by combining protein precipitation technology (PPT), efficiency lipid removal technology (ELR) and ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The OUVs include five benzophenone compounds, five benzotriazole compounds, two cinnamate ester compounds and their three metabolites, two salicylate compounds, two camphor derivative compounds, one triazine compound, one dibenzoylmethane compound and one amino aminobenzoic acid derivative compound. Chromatography was performed using an Acquity BEH C18 column (100 mm×2.1 mm, 1.7 μm), gradient elution was carried out using methanol-water and methanol-0.1% ammonia water as the mobile phases. Compounds were detected in both positive and negative electrospray ionization (ESI+/ESI) modes using multiple reaction monitoring (MRM), and quantified using stable-isotope internal standards. The experimental results showed that the 22 target compounds exhibited good linear relationships within their respective linear ranges, with the correlation coefficients (r)≥0.999 3. The method detection limits (MDLs) ranged from 0.02 to 0.48 ng/mL, and the method quantification limits (MQLs) ranged from 0.02 to 1.60 ng/mL. At the three spiked levels of low, medium and high, the spiked recoveries of the 22 target analytes ranged from 79.9% to 136.1%, the intra-day precisions were from 1.5% to 25.4%, and the inter-day precisions were from 0.6% to 23.5%. After correction by the stable-isotope internal standard method, the matrix effects of the 22 target analytes in fetal bovine serum were 83.0%‒119.9%. The developed method was successfully used to detect 22 OUVs in 110 human serum samples. With the exception of 3-benzylidene camphor (3-BC), 2-(2H-benzotriazol-2-yl)-4-methyl-6-(2-propenyl)phenol (UV-9), 4-methylbenzylidene camphor (4-MBC), 2,2'-dihydroxy-4-methoxybenzophenone (BP-8), and 2,4-dihydroxybenzophenone (BP-1), which were not detected, the remaining 17 substances were detected with overall detection rates of 0.9%-65.5% and the detection levels were

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超高效液相色谱-串联质谱法测定人血清中22种有机紫外吸收剂
本研究采用蛋白质沉淀技术(PPT)、高效去脂技术(ELR)和超高效液相色谱-串联质谱(UPLC-MS/MS)相结合的方法,建立了同时测定人血清中22种有机紫外吸收剂(OUVs)的方法。ouv包括五种二苯甲酮类化合物、五种苯并三唑类化合物、两种肉桂酸酯类化合物及其三种代谢物、两种水杨酸类化合物、两种樟脑衍生物、一种三嗪类化合物、一种二苯甲酰甲烷类化合物和一种氨基苯甲酸衍生物。色谱柱为Acquity BEH C18 (100 mm×2.1 mm, 1.7 μm),以甲醇-水和甲醇-0.1%氨水为流动相进行梯度洗脱。采用多反应监测(MRM)技术对正、负电喷雾电离(ESI+/ESI -)模式下的化合物进行检测,并采用稳定同位素内标进行定量。实验结果表明,22个目标化合物在各自的线性范围内呈良好的线性关系,相关系数(r)≥0.999 3。方法检出限为0.02 ~ 0.48 ng/mL,定量限为0.02 ~ 1.60 ng/mL。在低、中、高3个加标水平下,22种目标物的加标回收率为79.9% ~ 136.1%,日内精密度为1.5% ~ 25.4%,日内精密度为0.6% ~ 23.5%。经稳定同位素内标法校正后,22种靶物在胎牛血清中的基质效应为83.0% ~ 119.9%。该方法成功地检测了110份人血清样品中的22种ouv。除3-苄基樟脑(3-BC)、2-(2h -苯并三唑-2-基)-4-甲基-6-(2-丙烯基)苯酚(UV-9)、4-甲基苄基樟脑(4-MBC)、2,2′-二羟基-4-甲氧基二苯甲酮(BP-8)和2,4-二羟基二苯甲酮(BP-1)未检出外,其余17种物质均检出,总检出率为0.9% ~ 65.5%,检出水平为
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