Aswania O A, Corlett S A, Chrystyn H
Postgraduate Studies in Pharmaceutical Technology, School of Pharmacy, University of Bradford, UK.
J Chromatogr B Biomed Sci Appl. 1997 Mar 7;690(1-2):373-8. doi: 10.1016/s0378-4347(96)00382-9.
An ion-pair liquid high-performance chromatography method with solid-phase extraction for measuring urinary concentrations of sodium cromoglycate following inhalation has been developed and validated. Sodium cromoglycate was extracted from urine on a 100-mg phenyl cartridge (Isolute, Jones Chromatography) and then quantified on a 25-cm C8 Spherisorb 5 microns stationary phase with a mobile phase of methanol-0.045 M phosphate buffer-0.05 M dodecyl triethyl ammonium phosphate (550:447.6:2.4, v/v) pH 2.3, at 0.85 ml min-1 using nedocromil sodium as an internal standard and UV detection at 238 nm. The inter- and intra-day reproducibilities were 8.33 and 13.63%, respectively, at 0.25 mg l-1. The limit of determination for sodium cromoglycate was 0.25 mg l-1 (with a signal-to-noise ratio of greater than 10:1). Following oral and inhaled administration of 20 mg of sodium cromoglycate to eight healthy volunteers, the mean and S.D. of sodium cromoglycate excreted in the urine at 0.5, 1 and 24 h post-dose were 0.02, 0.05 and 0.33%, and 0.16, 0.30 and 1.55% of the dose, respectively. The urinary recovery of sodium cromoglycate at 0.5 and 1 h following inhalation can therefore be used to compare the amount of drug reaching the respiratory tract using different sodium cromoglycate inhaled products or inhalation methods.
已开发并验证了一种采用固相萃取的离子对液相高效色谱法，用于测定吸入后尿中色甘酸钠的浓度。色甘酸钠在100毫克苯基柱（Isolute，Jones色谱）上从尿液中萃取，然后在25厘米的C8 Spherisorb 5微米固定相上进行定量，流动相为甲醇-0.045 M磷酸盐缓冲液-0.05 M十二烷基三乙铵磷酸盐（550:447.6:2.4，v/v），pH 2.3，流速为0.85毫升/分钟，以内色奈甲酸钠为内标，在238纳米处进行紫外检测。在0.25毫克/升时，日间和日内重现性分别为8.33%和13.63%。色甘酸钠的测定限为0.25毫克/升（信噪比大于10:1）。对8名健康志愿者口服和吸入20毫克色甘酸钠后，给药后0.5、1和24小时尿中排出的色甘酸钠的平均值和标准差分别为剂量的0.02%、0.05%和0.33%，以及0.16%、0.30%和1.55%。因此，吸入后0.5和1小时色甘酸钠的尿回收率可用于比较使用不同色甘酸钠吸入产品或吸入方法到达呼吸道的药物量。
