乙基磺原酸钾—MIBK萃取原子吸收测定重晶石中铅,镉

本文较详细地研究了以乙基磺原酸钾作为金属分离的溶剂萃取试剂测定重晶石中铅，镉的条件，并确定了测定方法，铅和镉与乙基磺原酸钾反应生成白色络合物，该络合物在水相溶液中能定量地萃入甲基异丁基甲酮中。它们的回收率分别为９７％－１０３％和９６％－１０１％。铅和镉分别在０－６μｇ／ｍＬ和０－０．８μｇ／ｍＬ呈线性关系。本法可测定０．０００ｘ％－０．ｘ％Ｐｂ，０．０００ｘ％－０．０ｘ％Ｃｄ．     

中药片仔癀,六味地黄丸中的微量铬,铅和镉石墨炉原子吸收法测定

本文采用ＧＦ－ＡＡＳ加平台技术，基体改进剂，测定了中药片仔癀，六味地黄丸中铬、铅和镉的含量，铬、铅和镉的线性范围分别为０－０．８ｎｇ／ｍＬ，０－５０ｎｇ／ｍＬ，０－５ｎｇ／ｍＬ，回收率分别为１０２－１０３％，９９－１０１％，９７．５－９８％，本方法简便快速、准确。     

染料中间体二氰基─4─硝基苯胺的分析

应用薄层色谱（ＴＬＣ）和紫外光谱法（ＵＶ）对二氰基－４－硝基苯胺合成中涉及的主要产物进行分析。比传统化学法快速、简单、准确，回收率９９．１％～１０１．１％，相对标准偏差０．４８％～０．８５％，在０～６ｍｇ／Ｌ范围内遵守比耳定律。     

染料中间体二氰基─4─硝基苯胺的分析

应用薄层色谱（ＴＬＣ）和紫外光谱法（ＵＶ）对二氰基－４－硝基苯胺合成中涉及的主要产物进行分析，比传统化学法快速，简单，准确，回收率９９．１％～１０１．１％，相对标准偏差０．４８％～０．８５，在０～６ｍｇ／Ｌ范围内遵守比耳定律。     

反相离子对高效液相色谱法检测兔脑中的磷酸腺苷

采用反相离子对高效液相色谱法测定兔脑提取液中的磷酸腺苷。分别考察了流动相中ＴＢＡＨ，磷酸盐和甲醇的浓度对磷酸腺苷保留行为的影响。确认最佳色谱条件为甲醇２０％，２０ｍｍｏｌ／Ｌ ＫＨ２ＰＯ４－２ｍｍｏｌ／ＬＴＢＡＨ８０％，等度洗脱。保留时间和峰高的相对标准偏差分别为０．２９９％－０．４４３％和０．１８０％－０。．８９％；样品标准加入回收率为１０１．７２％－８６．３６％．最低检测限为ＡＭＰ０．２１，ｇ     

2—氰基—4—硝基苯胺的薄层色谱紫外光度分析

本文应用薄层色谱紫外光度法，测定了产品的主要成分２－氰基－４－硝基苯胺和杂质，得到了满意的分析结果。与经典化学法比较，这种方法具有简单、快速、精确的特点。回收率９９％－１０１％，相对标准偏差０．７％－１．１％，２－氰基－４－硝基苯胺含量在０－１３５μｇ／２５ｍＬ范围内遵守比耳定律。     

铜（Ⅰ）—苯骈三氮唑络合吸附波的极谱研究与应用

本文在０．６ｍｏｌ／Ｌ ＮＨ３－ＮＨ４Ｃｌ缓冲溶液（ｐＨ＝９．８）中，Ｃｕ（Ⅱ）在滴汞电极上还原生成Ｃｕ（Ⅰ），可与苯骈三氮唑（ＢＴＡ）络合，产生一灵敏的络合吸附波，Ｅｐ＝－０．７３Ｖ（ｕｓ，ＳＣＥ）。苯骈三氮唑的浓度在０．４０－１０．０ｍｇ／Ｌ范围内与极谱波峰高呈线性关系，检测下限为０．４０ｍｇ／Ｌ，相对标准偏差为１．４％－３．２％；回收率为９７．５％－１０１．５％。     

空气—C2H2火焰原子吸收光谱法测定中草药（鸦胆子,补骨脂）中…

用空气－Ｃ２Ｈ２火焰原子吸收光谱法测定了中草药中的Ｆｅ、Ｍｇ含量，讨论了测定条件，结果令人满意，方法的回收率：Ｆｅ９８．２０％－１０４．９％，ＣＶ１．０６％－１．０７％，Ｍｎ９９．４％－１０１％，ＣＶ＝０．５２％－１．９４％。     

离子交换分离—氢化物原子吸收光谱法测定紫铜中微是量硒

采用阳离子交换树脂离子分离铜，发生氢化物原子吸收光谱法测定硒，上柱溶液酸度在０－７％，硒的回收率在９６－１０１％，过柱溶液中铜的浓度低于０．０１μｇ／ｍＬ。方法检出限为５×１０＾－５％，分析紫铜中４．４×１０＾－４％的硒，相对标准偏差为３％。     

2－氰基－4－硝基苯胺的薄层色谱紫外光度分析

本文应用薄层色谱紫外光度法，测定了产品中的主要成分２－氰基－４－硝基苯胺和杂质，得到了满意的分析结果。与经典化学法比较，这种方法具有简单、快速、精确的特点。回收率９９％～１０１％，相对标准偏差０．７％～１．１％，２－氰基－４－硝基苯胺含量在０～１３５μｇ／２５ｍＬ范围内遵守比耳定律。     

芹菜籽香气成分研究

采用固相微萃取法萃取黑龙江产芹菜籽香气成分,然后用GC—MS进行成分分析,并与水蒸气蒸馏法获得的精油成分进行比较．用CAR on PDMS萃取柱进行顶空固相微萃取时,共检测出26种成分,鉴定出占总成份89．650％的20种成分,主要成分为柠檬烯（35．980％）,β-月桂烯（20．500％）,β-蛇床烯（16．160％）,正戊基苯（5．295％）,β-蒎烯（3．412％）,α-蛇床烯（3．293％）．水蒸汽蒸馏法提取芹菜籽,以1．18％产率获得精油,共检测出23个成分,鉴定出占总精油91．375％的18种成分,主要成分为柠檬烯（31．149％）,β-蛇床烯（22．281％）,对甲苯基异戊酸酯（14．944％）,α-2-丙烯基苯甲醇（9．872％）,β-月桂烯（4．324％）和α-蛇床烯（4．322％）．     

离子色谱法测定大豆木质部汁液中的Cl-、SO42-、NO3-、PO43-、柠檬酸和苹果酸

建立了离子色谱法测定大豆木质部汁液中Cl~-、SO_4~(2-)、NO_3~-、PO_4~(3-)、柠檬酸和苹果酸的方法。Cl~-、SO_4~(2-)、NO_3~-、PO_4~(3-)、柠檬酸和苹果酸的检出限分别为0.01、0.04、0.05、0.05、0.30和0.10 mg/L,相对标准偏差分别为8.34％、4.68％、9.54％、6.86％、5.52％和7.50％,线性范围分别为0.5～50.0、1.0～100.0、0.5～50.0、1.0～100.0、5.0～100.0和1.0～100.0 mg/L,回收率分别为103％～106.7％、92％～98.7％、93％～95.5％、91.7％～92％、93.2％～106％和94％～108.3％。方法简便、快速,测定结果准确,无干扰。     

X-射线荧光光谱法测定钛铁中的硅、锰、磷、铝

介绍用X-射线荧光光谱仪测定钛铁中Si、Mn、P、Al含量的方法,通过试验确定了合适的研磨时间、压力和保压时间,用压片法制样,建立了各元素的工作曲线,各元素的测定范围分别为Si3.00%～6.00%,Mn1.00%～3.00%,P0.030%～0.070%,Al5.00%～9.00%。通过强度测量得到测定Si、Mn、P、Al的相对标准偏差分别为0.074%、0.308%、0.383%、0.040%,精密度满足测试要求。将该方法测定结果与化学法比对,准确度满足国家标准方法分析误差的要求。     

固相微萃取-气相色谱-质谱法分析香樟籽挥发性成分

采用固相微萃取-气相色谱-质谱法分离和鉴定香樟籽的挥发性成分,用归一化法测定其相对含量。共分离出76种组分,鉴定出47种化合物,其含量占总挥发性成分的97.4%。主要挥发成分为樟脑(57.89%)、柠檬烯(12.68%)、α-蒎烯(4.42%)、莰烯(2.69%)、香橙烯(2.34%)、伞花烃(2.26%)及β-蒎烯(2.12%)。     

美白祛斑化妆品中镉、锰、铜、锌的原子吸收光谱法测定

将美白祛斑化妆品在硝酸-过氧化氢或硝酸-过氧化氢-氢氟酸体系中经微波消解后,用原子吸收光谱法测定其中的镉、锰、铜、锌含量。结果表明,在特定的测定工作条件下,镉、锰、铜、锌分别在2.0、3.0、6.0、2.0 mg.L-1内与吸光值呈现良好的线性,其检出限分别为2.6、2.8、19.0、2.6μg.L-1(n=20)。该法用于测定美白化妆品的镉、锰、铜、锌元素上线性好,回收率高,分别在98.3%～101.2%、99.0%～102.7%、98.0%～101.3%、99.0%～103.0%,精密度好,其RSD分别为3.4%、5.5%、3.5%、4.7%(n=6)。     

Essential oil composition of Erica spiculifolia Salisb - first report

The essential oil isolated from Erica spiculifolia Salisb. by hydrodistillation was analysed by GC-MS. One hundred compounds representing 92.6% of total oil were identified. Among the detected compounds 38 were monoterpenoids (46.2%), 30 were sesquiterpenoids (31.7%), 2 diterpene (0.4%) and 30 compounds (14.3%) were with various non-terpenoid structures. Oxygenated monoerpenes were by far the main class (45.3%) with α-terpineol (7.5%) endo-borneol (7.2%), pinocarveol (5.9%) and thymol (3.7%) as the major compounds. The predominant components of sesquiterpenes were caryophyllene oxide (5.0%), caryophyllene (4.2%), τ –murrolol (3.5%), spathulenol (2.9) and α-cadinol (2.3%).     

气相色谱-质谱法测定蒜头果油中的脂肪酸

 对云南产蒜头果油用硫酸 甲醇法酯化 ,以气相色谱 质谱 计算机联用仪进行了分析。共分离出 17种成分 ,鉴定了其中的 7种成分 ,分别为棕榈酸 (质量分数 (下同 ) 1.5 0 % )、油酸 (2 1.5 4% )、二十碳烯 11 酸 (7.0 4% )、芥酸(18.2 9% )、二十二烷酸 (1.33% )、二十四碳烯 15 酸 (4 0 .92 % )、二十四烷酸 (2 .14% ) ,占总质量的 92 .76 % ;未被鉴定的成分占总质量的 7.2 4%。     

两种水产品中农药多残留分析的样品前处理方法及其在111种农药和相关化学品残留同时检测中的应用

建立了两种针对水产品中农药多残留分析的快速样品前处理方法,并将其应用于111种农药及相关化学品残留检测。在样品前处理方法Ⅰ中,样品经丙酮-乙酸乙酯-正己烷(体积比为1∶1∶1)混合溶剂提取,乙腈转溶;在样品前处理方法Ⅱ中,样品用乙腈-水溶液均质,超声波辅助提取,液-液分配。两种方法所得到的提取液分别用Envi-18柱和PSA柱净化后进行气相色谱-质谱(GC-MS)分析。采用选择离子扫描(SIM)方式,外标法定量。该方法简便、快速,在优化的样品前处理条件和GC-MS分析条件下,方法的检出限(S/N=3)为0.001～0.026 mg/kg;在加标水平为0.25 mg/kg时,采用方法Ⅰ时的回收率为72%～113%,相对标准偏差（RSDs）为3.4%～12.1%;采用方法Ⅱ时的回收率为51%～127%(其中回收率为70%～120%的占94%),RSDs为3.2%～13.8%。     

Effect of certain chemical compounds on secondary metabolites of Penicillium janthinellum and P. duclauxii

The secondary metabolites of Penicillium janthinellum and P. duclauxii were affected by different concentrations of cadmium nitrate, sodium chloride, and sucrose. The fungal culture characteristics including mycelial fresh and dry weight, colony diameter, colony spore mass and reverse color, number of spores, and secondary metabolites were affected as well. Cyclopenin, carlosic acid, erythroskyrin, kojic acid, and patulin were produced by P. janthinellum on cadmium nitrate-free medium. However, cyclopenin, carlosic acid, frequentin, and islandicin were produced at 100 ppm, and cyclopenin at 500 ppm. On the other hand, the secondary metabolites produced by P. duclauxii were 9 on cadmium nitrate-free medium, 7 on medium containing 100 and 500 ppm of cadmium nitrate, and 4 at 1000 ppm cadmium nitrate concentration. Secondary metabolite brevianamide A was produced in the presence and absence of cadmium nitrate. The duclauxin, patulin, terrestic acid, and xanthomegin were produced only on cadmium nitrate-free medium. However, mycophenolic acid was produced only on cadmium nitrate-containing medium. The kojic acid was produced by P. janthinellum at 0.0%, 0.5%, 1.0%, 2.0%, 3.0%, and 5.0% concentrations of sodium chloride. The carlosic acid, erythroskyrin, and patulin were produced only at 0.0% and 1.0%. While carolic acid and islandicin were produced at 1%, 2%, and 3% and frequentin was produced only at 2% and 3%. On the other hand, 8 secondary metabolites were produced by P. duclauxii at 0.0%, 0.5%, 1.0%, and 2.0% concentration of sodium chloride and only 4 were produced at 3%. The secondary metabolites produced by P. janthinellum were 7 at 10% and 20%, 6 at 30%, and 2 only at 40% concentrations of sucrose. However, 8 secondary metabolites were produced by P. duclauxii at 10%, 20%, 30% and 3 at 40% concentrations of sucrose.     

High-throughput measurements of ciprofloxacin,clomipramine and fexofenadine hydrochlorides with an 8-channel electrical titrator

By employing a developed automatic eight-channel electrical titrator, ciprofloxacin, clomipramine and fexofenadine hydrochlorides are determined in batch, respectively, with satisfactory accuracy and precision. It shows a higher efficiency superior to traditional titration method, and maximally 30 measurements per minute can be completed.