Kintz P, Cirimele V, Dumestre-Toulet V, Ludes B
Institut de Médecine Légale, Universite Louis Pasteur, 11 rue Humann, F-67000 Strasbourg, France.
J Pharm Biomed Anal. 2001 Mar;24(5-6):1125-30. doi: 10.1016/s0731-7085(00)00570-7.
A sensitive, specific and reproducible method for the quantitative determination of nandrolone in human hair has been developed. The sample preparation involved a decontamination step of the hair with methylene chloride. The hair sample (about 100 mg) was solubilized in 1 ml NaOH IN, 15 min at 95 degrees C, in presence of 10 ng nandrolone-d(3) used as an internal standard. The homogenate was neutralized and extracted using consecutively a solid phase (Isolute C18) and a liquid--liquid (pentane) extraction. The residue was derivatized by adding 50 microl MSTFA/NH4I/2-mercaptoethanol (1000:2:5; v/v/v), then incubated for 20 min at 60 degrees C. A 4-microl aliquot of the derivatized extract was injected into the column (HP5-MS capillary column, 5% phenyl--95% methylsiloxane, 30 m x 0.25 mm i.d. x 0.25 mm film thickness) of a Hewlett Packard (Palo Alto, CA) gas chromatograph (6890 Series) via a Hewlett Packard (7673) autosampler. The assay was capable of detecting 0.5 pg of nandrolone per mg of hair when approximately 100 mg of hair were processed. Linearity was observed for nandrolone concentrations ranging from 1 to 50 pg/mg with a correlation coefficient of 0.997. Intra-day and between-day precisions at 10 pg/mg were 11.2 and 15.1%, respectively, with an extraction recovery of 81.7%. The analysis of three strands of hair, obtained from three bodybuilders, revealed the presence of nandrolone at the concentration of 1, 3.5 and 7.5 pg/mg.
已开发出一种灵敏、特异且可重复的方法，用于定量测定人发中的诺龙。样品制备包括用二氯甲烷对头发进行去污步骤。将头发样品（约100毫克）在1毫升1N氢氧化钠中，于95℃下在10纳克诺龙-d(3)作为内标的情况下溶解15分钟。将匀浆中和，然后依次使用固相（Isolute C18）和液-液（戊烷）萃取进行提取。通过加入50微升MSTFA/NH4I/2-巯基乙醇（1000:2:5；v/v/v）对残渣进行衍生化，然后在60℃下孵育20分钟。取4微升衍生化提取物注入惠普（加利福尼亚州帕洛阿尔托）气相色谱仪（6890系列）的色谱柱（HP5-MS毛细管柱，5%苯基-95%甲基硅氧烷，30米×0.25毫米内径×0.25毫米膜厚）中，通过惠普（7673）自动进样器进样。当处理约100毫克头发时，该测定法能够检测出每毫克头发中0.5皮克的诺龙。诺龙浓度在1至50皮克/毫克范围内呈线性，相关系数为0.997。在10皮克/毫克时，日内和日间精密度分别为11.2%和15.1%，提取回收率为81.7%。对从三名健美运动员处获得的三缕头发进行分析，发现诺龙浓度分别为1、3.5和7.5皮克/毫克。
