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超高效液相色谱-串联质谱法快速同时测定掺假产品中12种毛发生长化合物的方法的建立与验证

Development and validation of rapid and simultaneous method for determination of 12 hair-growth compounds in adulterated products by UHPLC-MS/MS.

作者信息

Park Han Na, Lee Ji Hyun, Park Sung-Kwan, Baek Sun Young, Lee Yong-Moon, Kang Hoil

机构信息

Division of Advanced Analysis, Toxicological Evaluation and Research Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Cheongju-si, Chungcheongbuk-do 28159, Republic of Korea.

Division of Advanced Analysis, Toxicological Evaluation and Research Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Cheongju-si, Chungcheongbuk-do 28159, Republic of Korea; College of Pharmacy, Chungbuk National University, Cheongju-si, Chungcheongbuk-do 28159, Republic of Korea.

出版信息

Forensic Sci Int. 2018 Mar;284:129-135. doi: 10.1016/j.forsciint.2017.12.042. Epub 2018 Jan 8.

Abstract

Synthetic hair-growth compounds have been illegally used in diverse products to enhance the short-term efficacy of these products. In this study, a rapid and simultaneous method for the determination of hair-growth compounds in adulterated products based on ultra high pressure liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was developed and validated. The limit of detection (LOD) and limit of quantitation (LOQs) of the method were 0.08-43.6ng/mL and 0.27-145ng/mL for the solid-, liquid-, and cream-type samples, respectively. Good calibration linearity for all compounds was demonstrated with a correlation coefficient (r) higher than 0.997. The intra- and inter-assay precisions were within 11%. The corresponding accuracies were 86-117% and 81-113%, respectively. The mean recoveries obtained for the solid-, liquid, and cream-type samples ranged from 87 to 114%, with a relative standard deviation (RSD) within 6%. The RSD of the stability evaluated at 4°C for 48h was less than 6%. The established method was used to screen 76 samples advertised as hair-growth treatments, from online and offline markets, over the course of two years. In 10% of the samples, four compounds, including triaminodil, minoxidil, finasteride, methyltestosterone, and testosterone-propionate were detected. The concentrations were in the range of 0.5-16.4mg/g. This technique provides a reliable platform for technical analysis for continuous monitoring of adulterated products to protect public health.

摘要

合成生发化合物被非法用于各种产品中,以提高这些产品的短期功效。在本研究中,开发并验证了一种基于超高压液相色谱-串联质谱法(UHPLC-MS/MS)快速同时测定掺假产品中生发化合物的方法。该方法对固体、液体和乳膏型样品的检测限(LOD)和定量限(LOQ)分别为0.08 - 43.6ng/mL和0.27 - 145ng/mL。所有化合物均显示出良好的校准线性,相关系数(r)高于0.997。批内和批间精密度均在11%以内。相应的准确度分别为86 - 117%和81 - 113%。固体、液体和乳膏型样品的平均回收率为87%至114%,相对标准偏差(RSD)在6%以内。在4°C下评估48小时的稳定性RSD小于6%。在两年的时间里,使用所建立的方法对从线上和线下市场收集的76个宣称有生发功效的样品进行了筛查。在10%的样品中,检测到了四种化合物,包括曲安奈德、米诺地尔、非那雄胺、甲基睾酮和丙酸睾酮。浓度范围为0.5 - 16.4mg/g。该技术为持续监测掺假产品以保护公众健康提供了一个可靠的技术分析平台。

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