腹泻性贝毒的高效液相色谱法测定条件改进及其运用

对腹泻性贝毒的高效液相色谱测定方法的条件进行改变，使原来对实验条件要求苛刻的方法更适宜于一般的实验室使用，使其有可能替代国内目前常用的小鼠生物方法。井成功地运用于冬季大连海域贝类腹泻性贝毒的检测，首次报道了大连地区海域贝类腹泻性贝毒的主要成分大田软海绵酸的含量，其结果是2000年1—3月大连地区海域贝类腹泻性贝毒除个别海区外一般都末检出。     

低浓度磷酸一酯的膜富集和气相色谱测定

磷酸一酯（ＲＯ）Ｐ（Ｏ）（ＯＨ）２是一种强极性的有机磷化合物。研究了水体中磷酸一（１－萘）酯的富集和上色谱分析,建立了一个简便快速、高灵敏度、实用的分析方法。富集是采用固相萃取方法,选用载有十八烷基硅烷的尼龙滤膜吸附,甲醇洗脱,回收率达７２％￣７％。它的气相色谱分析选用ＢＳＴＦＡ为衍生剂,反应条件为温度６５℃,反应时间３０ｍｉｎ,获得了满意的结果。方法的最低检测限为０。０６ｎｇ。     

Lignin in marine environment and its analysis—A review

Lignin is a group of phenolic polymers which is abundant in the woody tissues of vascular plants,and is essentially absent from all other living organisms.It has therefore been accepted as a tracer for terrestrial organic carbon(TOC) in marine environment since the 1970s.Lignin polymers are not amenable to direct chemical analysis without prior isolation.This review focused on the methods of chemical decomposition,extraction,derivatization and detection of lignin in marine environment.We described and compared several chemical decomposition methods,including nitrobenzene oxidation,alkaline cupric oxide(CuO) oxidation and thermochemolysis,and detection methods such as gas chromatography(GC),gas chromatography-mass spectrometry(GC-MS),high performance liquid chromatography(HPLC) and so on.Possible improvement of lignin analysis and the application prospects of this tracer were also discussed.     

Oxygen-containing functional groups in land-derived humic acids—I. Evaluation by derivatization methods

Determinations of reactive oxygen-containing functional groups were performed by usual chemical derivatization methods of four humic acids isolated from soils and deltaic sediments. Statistical tests and calculations based on elemental analysis demonstrated the validity and limits of these techniques and allowed us to identify from 60 to 71% of the total humic oxygen. Oxygen budgets of humic acids are discussed.     

Oxygen-containing functional groups in land-derived humic acids—II. Changes in the oxygen distribution of humic acids during early diagenesis as revealed by derivatization methods

Extensive functional group analyses were performed on humic acids representative of eight increasing depth levels from a core drilled in the Mahakam delta (East Kalimantan, Indonesia). Oxygen amounts decrease observed during early diagenesis was related chiefly to loss of hydroxyl (lignol?) groups. Comparison between upper and deeper levels shows the following variations: hydroxyl group abundances go from 19 to 6% of humic oxygen. Identified functional groups amounts represent 47 to 32% of weight of moisture- and ash-free humic acids. No evidence of decarboxylation of humic material was detected.     

两种氨基酸衍生化方法的比较研究

氨基酸的衍生化过程是气相色谱-燃烧-同位素比值质谱法(GC/C/IRMS)测定单体氨基酸碳稳定同位素组成方法中的关键步骤之一。采用了2种氨基酸衍生化方法分别对17种标准氨基酸进行衍生化处理：一种是氨基酸N-乙酰基正丙酯(NAP)法,另一种是氨基酸N-三氟乙酰基异丙酯(TFAIP)法。通过测量17种氨基酸衍生化前后的稳定碳同位素组成,比较了每种方法的重复性及衍生化过程中的同位素分馏作用的大小。结果说明氨基酸N-三氟乙酰基异丙酯(TFAIP)法是一种较为理想的氨基酸衍生化方法。     

柱前衍生-气相色谱法同时测定水中醛酮类和硝基苯类化合物

建立了柱前衍生-气相色谱法同时测定水样中醛酮类及硝基苯类化合物含量的检测方法。对影响衍生效率的因素如溶液的酸度、反应温度和时间、衍生试剂2,4-二硝基苯肼(DNPH)的用量等因素进行了试验,确定了DNPH与醛酮类化合物反应生成腙的最佳条件为pH=3时40℃恒温水浴反应1h。利用二氯甲烷萃取反应生成的腙和硝基苯类化合物,旋转蒸发仪浓缩,氮吹转换甲醇相,使用电子捕获检测器的气相色谱仪测定目标化合物。各化合物的质量浓度与其色谱峰峰面积的线性相关系数均在0.9989以上,方法检出限为0.01～0.03μg/L,相对标准偏差(RSD,n=6)均低于6.0%,回收率在89.5%～110.2%。方法简便、经济、回收率高,可用于水质中醛酮类及硝基苯类化合物的检测。     

DABS—C1柱前衍生高效液相色谱法测定对虾肌肉中18种游离氨基酸

建立一种以DABS-Cl为柱前衍生剂，利用反相高效液相色谱测定对虾肌肉中18种游离氨基酸的方法。结果表明，在50min内18种氨基酸得到完全分离，各氨基酸相关系数均大于0．997，氨基酸的回收率在86．60%-107．27％之间（胱氨酸除外），方法的检出限为0．18~o．66mg／L，相对标准偏差为3．53％-8．51％（天冬氨酸除外）。     

邻苯二甲醛柱前衍生高效液相色谱法测定马氏珠母贝中牛磺酸含量

应用邻苯二甲醛柱前衍生高效液相色谱法,测定了马氏珠母贝中牛磺酸,结果表明:采用邻苯二甲醛为柱前衍生剂,与原料中的牛磺酸发生衍生化反应后,以甲醇-乙酸钠溶液(体积比40︰60)为流动相,使用ODSC18分离柱,FLD检测器(EX=338nm,EM=444nm)等色谱条件下检测,牛磺酸的线性范围为2.0～14.0μg/mL,相关系数R2为0.9984,回收率为97.9%～103.0%,RSD=2.146%(n=6),检出限为0.77μg(S/N=3)。