Cieri Ugo R
US Food and Drug Administration, 2nd and Chestnut Sts, Philadelphia, PA 19106, USA.
J AOAC Int. 2003 Nov-Dec;86(6):1128-34.
A liquid chromatographic (LC) method with 2 detection systems for determining atropine (hyoscyamine) sulfate in commercial products was tested in a multilaboratory study. Depending on the type of product, sample solutions are prepared in methanol or methanol-water (1 + 1). The standard solution contains about 1.0 mg atropine sulfate/100 mL and is prepared in the same solvent used in sample preparation. LC separations are performed on a 7.5 cm Novapak silica column. The mobile phase is prepared by mixing 970 mL methanol with 30 mL of a 1% aqueous solution of 1-pentanesulfonic acid, sodium salt. Detection is by 2 systems, UV absorbance detection at 220 nm and fluorescence detection with excitation at 255 nm and emission at 285 nm. The injection volume is 100 or 200 microL. The following materials were used for the study: 2 separate samples of tablets labeled to contain 0.4 mg atropine sulfate, 2 separate samples of extended-release tablets labeled to contain 0.375 mg hyoscyamine sulfate, one sample of atropine sulfate injection labeled to contain 2 mg/mL, and one sample of 1% (v/v) atropine sulfate ophthalmic. Eight participants analyzed 2 separate portions of the 6 samples by both detection systems. A ninth participant analyzed the samples in duplicate but only by UV absorbance detection because of the unavailability of a fluorescence detector. The relative standard deviation (RSD) between laboratories ranged from 1.4 to 3.3% for samples of tablets and injections but higher for ophthalmic solutions (5.1-5.2%). A linearity study was conducted in the originating laboratory before the multilaboratory study with 5 solutions ranging in concentration from 0.80 to 1.20 mg atropine sulfate in 100 mL. Average recoveries were 100.0% by UV absorbance detection and 99.9% by fluorescence detection; the RSDs were 1.1 and 1.2%, respectively.
一种带有2种检测系统的液相色谱（LC）方法用于测定市售产品中的硫酸阿托品（莨菪碱），该方法在一项多实验室研究中进行了测试。根据产品类型，样品溶液用甲醇或甲醇 - 水（1 + 1）配制。标准溶液含有约1.0 mg硫酸阿托品/100 mL，且用与样品制备相同的溶剂配制。LC分离在一根7.5 cm的诺瓦帕克硅胶柱上进行。流动相通过将970 mL甲醇与30 mL 1%的戊烷磺酸钠盐水溶液混合制备。检测通过2种系统进行，220 nm处的紫外吸光度检测以及激发波长为255 nm、发射波长为285 nm的荧光检测。进样体积为100或200 μL。该研究使用了以下材料：2份单独的标示含0.4 mg硫酸阿托品的片剂样品、2份单独的标示含0.375 mg硫酸莨菪碱的缓释片剂样品、1份标示含2 mg/mL硫酸阿托品注射液样品以及1份1%（v/v）硫酸阿托品眼药水样品。8名参与者通过两种检测系统分析了6个样品的2个单独部分。第9名参与者由于没有荧光检测器，仅通过紫外吸光度检测对样品进行了双份分析。片剂和注射液样品在各实验室之间的相对标准偏差（RSD）范围为1.4%至3.3%，但眼药水溶液的相对标准偏差更高（5.1 - 5.2%）。在多实验室研究之前，发起实验室用5种浓度范围为0.80至1.20 mg硫酸阿托品/100 mL的溶液进行了线性研究。紫外吸光度检测的平均回收率为100.0%，荧光检测的平均回收率为99.9%；RSD分别为1.1%和1.2%。
