固相萃取技术-HPLC测定复方甘草片中吗啡的含量

 报道了用ＳＥＰ－ＰＡＫＣ１８小预柱固相萃取技术和反相高效液相色谱法测定复方甘草片中微量吗啡含量的方法。对固相萃取条件进行了研究，最终选择１０％甲醇溶液为清洗溶液，７０％甲醇溶液为洗脱溶液，基本消除了干扰组分对测定的影响，色谱图背景吸收小，基线平稳。色谱柱为μ－ＢｏｎｄａｐａｋＣ１８柱，流动相为０．１ｍｏｌ／ＬＮａＨ２ＰＯ４溶液－甲醇（５１），检测波长为２８６ｎｍ。平均回收率为（１０１．２±１．５）％，ＲＳＤ为１．５％。

Determination of morphine in compound liquorice tablets by high performance liquid chromatography with SEP-PAK C18 cartridge pretreatment]

An efficient method combining SEP-PAK C18 cartridge solid phase extraction (SPE) with reversed-phase high performance liquid chromatography for the quantitation of morphine in the Compound Liquorice Tablet is presented. The tablets have been used for making expectoration easy and relieving cough for years. The tablet powder (approximately 1 tablet) was added into a stoppered centrifuge tube, and vertically extracted with 5 mL of 0.5% HAc for 5 min. After centrifugation the supernatant was transferred to a beaker and the extraction was repeated twice with 4 mL and then 3 mL of 0.5% HAc. Five millilitres of carbonate buffer (pH 8.9) was added to the combined extracts. A SEP-PAK C18 cartridge was pretreated by passing methanol and distilled water, using a glass syringe. The mixture was applied on it and allowed to flow through. The cartridge was washed first with 5 mL of 10% methanol solution and then the morphine was eluted with 4 mL of 70% methanol solution into a 5 mL volumetric flask and was finally diluted to volume with 70% methanol solution. Analysis was performed on a mu-Bondapak C18 column(300 mm x 4.6 mm i.d., 10 microns) with 0.1 mol/L NaH2PO4-methanol(5:1) as the mobile phase and detection at 286 nm. The average recovery of morphine was (101.2 +/- 1.5)% and RSD was 1.5%. The method is simple, rapid, accurate, and reproducible, and can be used in drug control.