Fullinfaw R O, Bury R W, Moulds R F
Department of Clinical Pharmacology and Therapeutics, Royal Melbourne Hospital, Parkville, Victoria, Australia.
J Chromatogr. 1988 Dec 9;433:131-40. doi: 10.1016/s0378-4347(00)80591-5.
We describe a liquid chromatographic screening procedure for the detection of stimulant laxatives in urine. A 2-ml urine sample was incubated with 500 U of beta-glucuronidase for 2 h at 60 degrees C. The sample was acidified with sodium acetate (pH 5.0) and extracted with 5 ml of an isopropanol-chloroform (1:9) mixture. The organic layer was cleaned up further by washing with 5 ml disodium hydrogen-phosphate (pH 7.5) before being transferred to a conical tube and evaporated to dryness. The residue was reconstituted in 100 microliters mobile phase and 3 microliters were injected onto a Hewlett-Packard Hypersil ODS (5 microns) column. The ultraviolet absorbance of the eluent was monitored at 225 nm. Rhein, bisacodyl diphenol, bisoxatin diphenol, phenolphthalein, bisacodyl, bisoxatin and danthron all eluted within 6 min. The screen was evaluated using urine specimens obtained from 19 patients who claimed they had taken one or more of the laxatives under consideration within the past 48 h. Only two patients who claimed to have taken Coloxyl and Danthron showed negative results. Eighteen of twenty laxatives (90%) taken by the patients were detected and their identity verified by plotting post-run ultraviolet spectra. We therefore conclude that the screen is sufficiently reliable to be of help in the early detection of surreptitious abusers of stimulant laxatives.
我们描述了一种用于检测尿液中刺激性泻药的液相色谱筛查程序。取2ml尿液样本，与500Uβ-葡萄糖醛酸酶在60℃下孵育2小时。样本用醋酸钠（pH 5.0）酸化，并用5ml异丙醇-氯仿（1:9）混合物萃取。有机层在用5ml磷酸氢二钠（pH 7.5）洗涤进一步净化后，转移至锥形管并蒸发至干。残渣用100微升流动相复溶，取3微升注入惠普Hypersil ODS（5微米）柱。在225nm处监测洗脱液的紫外吸光度。大黄酸、比沙可啶二酚、双醋氧苯酸二酚、酚酞、比沙可啶、双醋氧苯酸和丹蒽醌均在6分钟内洗脱。使用从19名患者采集的尿液样本对该筛查方法进行评估，这些患者声称在过去48小时内服用了一种或多种所考虑的泻药。只有两名声称服用了复方芦荟胶囊和丹蒽醌的患者检测结果为阴性。患者服用的20种泻药中有18种（90%）被检测到，通过绘制运行后紫外光谱验证了它们的身份。因此，我们得出结论，该筛查方法足够可靠，有助于早期检测出偷偷滥用刺激性泻药的人。
