Pichini Simona, Pellegrini Manuela, Pacifici Roberta, Marchei Emilia, Murillo Janeth, Puig Carme, Vall Oriol, García-Algar Oscar
Drug Research and Control Department, Istituto Superiore di Sanità, V.le Regina Elena 299, 00161 Rome, Italy.
Rapid Commun Mass Spectrom. 2003;17(17):1958-64. doi: 10.1002/rcm.1140.
A high-performance liquid chromatography (HPLC) method with mass spectrometric detection is described for determination of arecoline in newborn meconium, urine and cord serum, using pilocarpine as internal standard. The analytes were extracted from neonatal biological matrices with chloroform/isopropanol (95:5, v/v) at alkaline pH. Extracts were analyzed by HPLC coupled to an electrospray (ESI) interface and a quadrupole mass spectrometer. Chromatography was performed on a C(8) reversed-phase column using 10 mM ammonium acetate (pH 4.3)/acetonitrile (90:10, v/v) as mobile phase. The mass spectrometer was operated in selected ion monitoring mode. The method was validated over the concentration range 0.005-1.00 micro g/g meconium, 0.004-1.00 micro g/mL cord serum and 0.001-1.00 micro /mL urine. Mean recoveries ranged between 86.5 and 90.7% for arecoline in the different biological matrices, with precision always better than 10%. The quantification limits of arecoline were 0.005 micro g/g meconium, 0.004 micro g/mL cord serum, and 0.001 micro g/mL urine. The method was applied to the analysis of neonatal biological matrices to assess eventual fetal exposition to arecoline. Two newborns from Asian mothers who declared areca nut consumption presented arecoline in meconium with concentrations in the range 0.006-0.008 micro g/g; also the urine from one neonate tested positive for the drug.
描述了一种采用质谱检测的高效液相色谱（HPLC）方法，以毛果芸香碱为内标，用于测定新生儿胎粪、尿液和脐带血清中的槟榔碱。分析物在碱性pH条件下用氯仿/异丙醇（95:5，v/v）从新生儿生物基质中提取。提取物通过与电喷雾（ESI）接口和四极杆质谱仪联用的HPLC进行分析。色谱分离在C(8)反相柱上进行，使用10 mM醋酸铵（pH 4.3）/乙腈（90:10，v/v）作为流动相。质谱仪在选择离子监测模式下运行。该方法在0.005 - 1.00μg/g胎粪、0.004 - 1.00μg/mL脐带血清和0.001 - 1.00μg/mL尿液的浓度范围内进行了验证。槟榔碱在不同生物基质中的平均回收率在86.5%至90.7%之间，精密度始终优于10%。槟榔碱的定量限为0.005μg/g胎粪、0.004μg/mL脐带血清和0.001μg/mL尿液。该方法应用于新生儿生物基质的分析，以评估胎儿是否最终暴露于槟榔碱。两名亚洲母亲声称食用过槟榔的新生儿，其胎粪中槟榔碱浓度在0.006 - 0.008μg/g范围内；一名新生儿的尿液对该药物检测呈阳性。
