氯胺酮、去甲氯胺酮、氟胺酮3个苯环利定类物质的毛发质控样品制备研究

Study on preparations of hair quality control samples containing ketamine, norketamine and fluoroketamine

目的:探究氯胺酮、去甲氯胺酮、氟胺酮3个苯环利定类物质毛发质控样品的制备方法和规律,分析不同制备条件和贮存条件对毛发质控样品的性能影响。方法:通过比较空白毛发(不含氯胺酮、去甲氯胺酮和氟胺酮的毛发)浸泡在不同种类的浸泡溶剂、不同目标物(氯胺酮、去甲氯胺酮、氟胺酮)浓度、不同酸度的浸泡试液和不同空白毛发浸泡量等条件下制备的毛发质控样品中目标物含量,系统分析了不同制备条件对毛发质控样品性能的影响,并按照研究规律采用乙腈-DMSO(1∶1,含0.02 mol·L-1盐酸)为浸泡溶液,将空白毛发浸泡不同时间段制备含量覆盖面较广的毛发质控样品;采用高效液相色谱-质谱联用仪,应用BEH C18(100 mm×2.1 mm,1.7μm)色谱柱,在柱温40℃,以0.1%(v/v)甲酸水溶液(A)-0.1%(v/v)甲酸乙腈溶液(B)为流动相,梯度洗脱(0~9 min,5%B→100%B;9~11 min,100%B;11~11.1 min,100%B→5%B;11.1~13 min,5%B),流速0.4 mL·min-1,进样量1μL的色谱条件下测定毛发质控样品中目标物含量。同时考察了1 cm段和粉末(冷冻研磨)2种状态毛发质控样品的均匀性、不同贮存条件下(温度、湿度、光照等条件)短期和长期稳定性。结果:确定了不同制备条件对氯胺酮等3种苯环利定类物质毛发质控样品的影响规律,发现浸泡溶液种类、浓度、酸度对毛发质控样品性能有较明显的影响,浸泡量因素对空白毛发几乎没有影响。制备的高、中、低含量的氯胺酮等3种物质的毛发质控样品,在1 cm段状态和粉末状态下均有较好的均匀性,按照F检验法计算各样品的F值均<F(0.05(查表))(即3.02);且样品均较为稳定,在室温、冷藏或冷冻条件下贮存6个月期间监测各样品中目标物的含量,RSD均<12%,按照t检验法计算各目标物的t值均<t(0.05(4)查表)(即2.1318)。结论:本研究为相关毛发质控样品的制备条件提供了较为详尽的数据,为后续毛发质控样品的制备和贮存条件提供参考。

Objective:To explore the prepararation methods and rules of hair quality control samples which contained ketamine, norketamine or fluoroketamine, and the effects of different preparation and storage conditions on the performance of hair quality control samples. Methods:Different preparation conditions were compared, such as different types of soaking solutions, solutions with different target contents, different amount of blank hair etc. The performances of hair quality control samples which were prepared in different conditions were systematically analyzed, and eighteen kinds of hair quality control samples with different contents of targets and different forms were prepared according to the rules, ACN-DMSO(1∶1, v/v, added 0.02 mol·L^(-1) hydrochloric acid) was used to soak blank hair in different time periods to prepare hair quality control samples with a wide coverage. HPLC-MS/MS instruments and BEH C_(18)(100 mm×2.1 mm, 1.7 μm) column were used to test the content of targets in hair. Column temperature was 40 ℃, the mobile phases were aqueous solution with 0.1%(v/v) formic acid(A)-acetonitrile aqueous solution with 0.1%(v/v) formic acid(B), gradient elution(0-9 min, 5%B→100%B;9-11 min, 100%B;11-11.1 min, 100%B→5%B;11.1-13 min, 5%B, a flow rats of 0.4 mL·min^(-1), inject volume of 1 μL. The homogeneity, short term and long term stability in different storage conditions(temperature, humidity, light conditions, etc.) were also investigated. Results:The influences of different preparation conditions on the hair quality control samples were determined, soaking solutions had strong influences on the hair quality control samples, however the amount of blank hair had nearly no effects. All the samples prepared were uniform, F of each sample was lower than F_(0.05(table))(3.02) according to the F-test method, and all the samples were stable, during storage at room temperature, refrigerated or frozen conditions for 6 months, the contents of the target substances in each sample were monitored, all of RSDs were <12%, and the t values of each sample were < t_((0.05)(table))(2.131 8) according to the T-test method. Conclusion:This study provides preparation rules of hair quality control samples and also provides detailed reference data for subsequent preparation and storage of related hair quality control samples.