In this paper, an accurate and route method was developed to quantitative determine daidzein, genistein, glycitein, daidzin, glycitin, 6 "-Oacetyldaidzin, 6" -O-acetylglycitin and 6”-O-acetylgenistin contents in selected high and low isoflavones in nutrition supplements by on line liquid chromatography–atmospheric pressure chemical ionisation mass spectrometry (LC-APCI-MS). Improved extraction and hydrolysis methods of the isoflavones from three nutrition supplements were also studied and a rapid extraction method was developed. Comparison of different MS2 and MS3 spectra of isoflavones and some unknown compounds were also explored and proposed pathway fragments of nine isoflavones were first systematically suggested.

Analytical Milli high-speed counter-current chromatography (HSCCC) was used for the selection and optimization of the two-phase solvent system to separate flavonoids from the extracts of the seeds of Oroxylum indicum. The optimum solvent system obtained from Milli-CCC was also the best solvent system for preparative HSCCC and led to the successful separation of two crude flavonoids from the seeds of O. indicum by Lab/Prep (laboratory preparative) HSCCC using different sized coils. Four flavonoids were isolated by preparative HSCCC: baicalein-7-O-diglucoside (25.0mg, 92% purity), baicalein-7-o-glucoside (50.4mg; 95% purity), baicalein (75mg; purity 98%) and chrysin (100 mg; purity 98%).

Four flavonoids, chrysin, baicalein, baicalein-7-O-glucoside, baicalein-7-O-diglucoside (Oroxylin B) and one unknown flavonoid have been isolated and purified for the first time in the seeds of Oroxylum indicum by high-speed counter-current chromatography with a two-phase solvent system composed of chloroform-methanol-water (8:10:5, v/v). Then, 50 mg baicalein-7-O-glucoside, 10.5mg baicalein-7-O-diglucoside, 4.5mg chrysin-7-O-diglucoside, 25 mg baicalein and 45 mg chrysin could be obtained after injecting 20 mg/ml sample extract ten times and their purities were 96, 90, 85, 95 and 98%, respectively. All these constituents were identified by high-performance liquid chromatography–mass spectrometry and nuclear magnetic resonance.

采用分光光度法，以重铬酸钾为显色剂，在1mol/L盐酸介质中不经分离测定复方乙酰水扬酸片、去痛片中非那西丁含量，其平均回收率和相对标准偏差分别为100.6%，0.36%；100.1%，0.26%，结果较满意。

对无水氯化钙与液氨的反应产物（简称CAC）的稳定性进行了研究，提出了改进CAC稳定性新技术—碳化法原位成盐包膜技术。研究表明：碳化法原位成盐包膜可以较好地提高CAC的稳定性。包膜CAC的最佳条件是：当CAC呈膏状且不流动时通以流速为120mL/min的CO2.3～5min对CAC进行微粒包膜，经造粒后进行大颗粒二次包膜。二次包膜后的CAC在25～35℃范围可以较稳定存在，且包膜后的CAC含氮量可以稳定在31%以上。大颗粒包膜CAC对其稳定性的增强更有利。

A highly sensitive spect rophotomet ric method for determination of selenium (Ⅳ) has been developed. It has been based on Se (Ⅳ) oxidation of I-in a weak acid medium and formation of the 1:1 ion-associatin complex of I-with Butylrhodamine B in the presence of poly (vinyl alcohol). The wavelength of maximum absorbance of this complex was at 590nm, The molar absorptivity was 2.57×105L.mol-1•cm-1 and Beer's law was obeyed in the concent ration range of 40～500ng/mL. The detection limit was 40ng/mL. Interfering ions were eliminated by using thiohydroxy cotton so that the selectivity of this method was good. The color system was used to determine the microamounts of Se in the liver of dophine and huangqi. Satisfactory result s were obtained.

有机锗具有提高人体免疫机能、降低血脂、抗癌、防癌及防衰老等多种功能。许多植物如人参、枸杞、茶叶、蘑菇中都含有有机锗，有些含锗食品已被国家批准为新资源性食品并引起人们的重视。对人参、枸杞中锗的测定方法较多，但对蘑菇中锗的测定还未见报道。蘑菇以其味美价廉深受人们喜爱，因此在研究蘑菇中有机锗的化学形态和结构的前提下，准确测定有机锗的含量对于新资源食品开发、利用及监测具有重要的意义。锗的测定方法多采用原子吸收法[1]和分光光度法[2～6]，分光光度法中常采用锗钼杂多酸一碱性染料离子缔和物显色法[1]和荧光酮比色法[4]，但由于铋（Ⅴ）、锑（Ⅲ）、钒（Ⅴ）等干扰元素的存在，两者常需萃取分离后才能测定。我们利用水杨基荧光酮作显色剂，在抗坏血酸、混合表面活性剂、聚乙烯醇存在下形成胶束体系，提高锗一水杨基荧光酮分光光度法的灵敏度，同时也消除了铋（Ⅴ）、锑（Ⅲ）、钒（Ⅴ）等离子的干扰，从而建立了灵敏度较高、选择性较好的测定植物中有机锗含量的方法。用该法测定人参、枸杞、茶叶、蘑菇中有机锗含量，结果满意。

亮氨酸、赖氨酸、缬氨酸、苯丙氨酸和蛋氨酸是人体必需组分，但却不能在体内合成，只能从食物中摄取[1]。由于这几种氨基酸与茚三酮显色反应的吸收光谱严重重叠，因而直接分光光度法测定其混合体系是不可能的。利用化学计量学不经分离同时分光光度测定氨基酸混合物曾有报道[2～6]引，而PLS法多用于无机混合物的分析[7～9]。我们通过校准模型的选择，利用PLS分光光度法同时测定了上述5种氨基酸混合物，结果与氨基酸自动分析仪所测一致，且较卡尔曼滤波法（KF）优越。这表明PLS法对处理光谱重叠严重、吸光度加和性尚可的体系效果较好，是一种计算简单而有效的数据处理方法。

In th is paper, the con ten t of phenacet in in compound tab let s of A sp irin, A n tongding and Keganm ing w ere determ ined in hydrogen ch lo ride acid by spect ropho tom et ry w ithou t any p relim inary separat ion. The po tassiun dich rom ate (0.1molL/L)w as adop ted as co llo r reagen t. The average recoverys and relat ive standard deviat ion s of compound A sp irin, A n tongding and Keganm ing tab let s are 100.6%, 0.355%, 100.1%, 0.263%, 99.27%, 0.598%, respect ively. Th is m ethod is simp le, rap id and w ith sat isfacto ry resu lt s.

对硒-碘化钾-结晶紫-聚乙烯醇显色体系进行了较系统的研究。结果表明，硒在盐酸介质中可与I3离子形成三元缔合物，其缔合物的最大吸收波长为560nm，E为2。31×105，硒含量在0～6μg/25ml范围内服从比耳定律，利用巯基棉分离干扰离子，选择性高，测定海豚肝脏及茶叶中硒含量与加标回收率，结果满意。