Hadad Ghada M, Abdel-Salam Randa A, Emara Samy
Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, University of Suez Canal, Ismailia 41522, Egypt.
J Chromatogr Sci. 2012 Apr;50(4):307-15. doi: 10.1093/chromsci/bms008. Epub 2012 Feb 23.
A simple and reliable precolumn derivatization liquid chromatography method with ultraviolet detection has been developed and validated for the analysis of glucosamine (GS) in various dietary supplement formulations and raw materials. Additionally, the proposed method was used for analysis of carisoprodol (CR) found in ternary mixture with paracetamol (PR) and caffeine (CF). The linearity ranges were 1-100 μg/mL for GS, 1-150 μg/mL for CR, PR and CF. Derivatization was used with 1,2-naphthoquinone-4-sulphonic acid sodium salt in the presence of borate buffer. Chromatographic separation of GS-naphthoquinone derivative was achieved by using a mixture of acetonitrile and water (pH 7.3 adjusted with 0.1 M NaOH) in the ratio 10:90, v/v and flow-rate of 1.0 mL/min. UV detection was carried out at 280 nm. For PR, CF, and CR-naphthoquinone derivative, the chromatographic separation was achieved by using mixture of acetonitrile and 20 mM KH(2)PO(4) (pH 3.0 adjusted with phosphoric acid) in the ratio 20:80, v/v and flow-rate of 1.0 mL/min. UV detection was carried out at 275 nm. The limits of detection were 37.2, 35.9, 30.4 and 40.0 ng/mL for GS, CR, PR and CF, respectively.
已开发并验证了一种简单可靠的柱前衍生化液相色谱法，用于紫外检测各种膳食补充剂配方和原料中的氨基葡萄糖（GS）。此外，该方法还用于分析在与对乙酰氨基酚（PR）和咖啡因（CF）的三元混合物中发现的卡立普多（CR）。GS的线性范围为1 - 100μg/mL，CR、PR和CF的线性范围为1 - 150μg/mL。在硼酸盐缓冲液存在下，使用1,2 - 萘醌 - 4 - 磺酸钠盐进行衍生化。通过使用体积比为10:90的乙腈和水（用0.1M NaOH调节pH至7.3）的混合物，流速为1.0 mL/min，实现GS - 萘醌衍生物的色谱分离。在280nm处进行紫外检测。对于PR、CF和CR - 萘醌衍生物，通过使用体积比为20:80的乙腈和20 mM KH₂PO₄（用磷酸调节pH至3.0）的混合物，流速为1.0 mL/min，实现色谱分离。在275nm处进行紫外检测。GS、CR、PR和CF的检测限分别为37.2、35.9、30.4和40.0 ng/mL。
