毛细管气相色谱法测定羟乙基淀粉中2-氯乙醇的残留量

目的建立毛细管气相色谱法测定羟乙基淀粉中2-氯乙醇的残留量。方法采用毛细管气相色谱法。色谱柱为DM-WAX弹性石英毛细管柱(30 m×0.25 mm,0.25μm);载气为氮气;检测器为ECD;进样口和检测器温度均为250℃;柱温为程序升温,初始温度90℃,保持12 min,以每分钟20℃升温至120℃,保持2 min。结果2-氯乙醇质量浓度在14.30~119.2μg.L-1内线性关系良好,r=0.997 6;回收率为98.4%(n=9);检测限为9.54×10-3ng;定量限为2.86×10-2ng。结论本法灵敏度高,简单,易行,结果准确可靠,可为羟乙基淀粉的质量控制提供依据。     

气相色谱法测定缝合针线中2-氯乙醇残留量

目的建立测定缝合针线中2-氯乙醇残留量的气相色谱法。方法依照国际标准ISO10993-7的气相色谱法,采用FFAP石英弹性毛细管柱（30m×0.32mm×0.25μm）,进样口温度200℃,检测器温度250℃,柱箱温度110℃。进样量1μL,分流比3,柱流速1.5mL·min-1。结果该方法灵敏准确,2-氯乙醇检测限为10μg,在52.75~422μg范围内保持良好的线性关系,缝合针线中2-氯乙醇平均回收率为98.8%。结论该方法可以作为缝合针线中2-氯乙醇残留量的测定方法。     

GC测定马来酸伊索拉定原料中二氧六环和2-甲氧基乙醇残留量

目的建立GC测定马来酸伊索拉定原料中二氧六环和2-甲氧基乙醇的残留量。方法样品以二甲基甲酰胺溶解,色谱柱为HP-INNOWAX毛细管柱（30m×0．53mm,1μm）,检测器为氢火焰离子化检测器,柱温为程序升温,初始柱温为40℃,进样口温度为200℃,检测器温度为250℃。结果二氧六环和2-甲氧基乙醇分别在7．6～76μg·mL^-1和1．0～10gg·mL^-1内线性关系良好p分别为0．9999和0．9984）,平均回收率分别为94．7％（RSD=3．7％）和98．2％（RSD=3．9％）,检测限分别为0．9μg·mL^-1和0.3μg·mL^-1。结论本方法灵敏度高、准确度好,可用于马来酸伊索拉定原料中二氧六环和2-甲氧基乙醇的残留量测定。     

气相色谱法测定质粒DNA中乙醇和异丙醇残留量

目的:建立测定质粒 DNA 中乙醇和异丙醇残留量的方法。方法:顶空进样气相色谱法。色谱条件:DB-624石英毛细管柱(30 m×0.53 mm×3μm),柱温:60℃,气化室温度:120℃,FID 检测器,温度为300℃;进样分流比:1:50,载气 N_2(3.0mL·min~(-1))。结果:乙醇、异丙醇线性关系良好(相关系数均大于0.9999);最低检测浓度分别为0.00125 mg·mL~(-1)和0.00083 mg·mL~(-1);平均回收率分别为100.1%和100.9%;平均 RSD 分别为3.0%和1.5%。结论:该法简单快速,可用于质粒 DNA 中乙醇和异丙醇残留量的测定。     

气相色谱法测定硝苯地平缓释片中的乙醇残留量

目的 建立硝苯地平缓释片中乙醇残留量的测定方法.方法 采用毛细管柱,顶空气相色谱法,SGE-H2毛细管柱;柱温60℃,保持3 min,以N2为载气,分流比1:1;以水为溶剂;顶空平衡温度为75℃,平衡时间为30～60 min;进样口温度200℃;FID检测器,检测器温度250℃.结果 乙醇在10～200 μg/ml进样量范围内,与乙醇浓度与峰面积呈良好的线性关系(r=0.998 2),加样回收试验乙醇的平均回收率为101.5%,RSD为2.29%(n=9).结论 所建立的方法专属性好,简便准确,可用于检测硝苯地平缓释片中的乙醇残留溶剂.     

气相色谱法测定抗生素中2-乙基己酸残留量

建立测定抗生素中2-乙基己酸残留量的气相色谱法。采用3-环己丙酸作内标物,氮气为载气,色谱柱为HP-FFAP,柱温：150℃,进样口温度：200℃,检测器温度：300℃。结果：该测定方法具有良好的线性关系（r=0.9997）、重复性（RSD=0.9%）和平均回收率（100.5%）。能准确测定抗生素中2-乙基己酸的残留量。     

毛细管色谱法测定黄体酮中乙醇残留量

目的:建立气相色谱法,测定黄体酮中的残留溶剂乙醇的含量.方法:毛细管柱,以N2为载气,柱温30℃,FID检测.结果:乙醇在25～150μg/mL范围内,浓度与峰面积线性关系良好(r=0.997 7),平均回收率为99.0%.结论:该方法灵敏、简便、准确,重现性好,可很好地控制制剂中乙醇残留量.     

运用气相色谱法评价体外循环一次性血管路中2-氯乙醇残留量的安全性

目的建立评价体外循环一次性血管路中2-氯乙醇残留量安全性的方法。方法采用气相色谱法对体外循环一次性血管路中2-氯乙醇残留量进行测定,优化各种检测条件。结果该法的分离度在3．0以上,理论塔板数在10000以上,线性关系较好,相关系数r=0．9996,精密度试验的RSD为3．68％,重复性试验的RSD为3．11％,平均加样回收率为100．5％（RSD=4．12％）。结论本方法灵敏度高,重复性好,简便可行,可有效地评价该类产品2-氯乙醇残留量的安全性。     

气相色谱法测定盐酸阿莫地喹中乙醇及醋酸的残留量

摘 要 目的：建立气相色谱法测定盐酸阿莫地喹中乙醇及醋酸的残留量。 方法: 采用DB 1701毛细管柱（30 m×0.32 mm×1.00 μm）,以氢火焰离子化检测器（FID）检测,载气为氮气,流速1.0 ml·min-1,柱温采用程序升温,进样口温度为200℃,检测器温度为250℃。 结果: 乙醇、醋酸和空白溶剂能达到良好分离;乙醇、醋酸的浓度线性范围分别为5.021 1～502.117 3 μg·ml-1(r=1.000 0）及5.021 7～502.173 6 μg·ml-1(r=0.999 8）,平均回收率分别为101.04%(RSD=0.65%)及97.33%(RSD=1.83%)（n＝6）。 结论: 本方法简单、准确、灵敏度高、重复性好,适用于盐酸阿莫地喹中乙醇和乙酸残留量的测定。     

气相色谱法测定丁胺卡那霉素中乙醇的含量

气相色谱法测定丁胺卡那霉素中乙醇的含量重庆市药品检验所６３００１５龚士学王白露张锦程辉跃吴蔚丁胺卡那霉素（Ａｍｉｋａｃｉｎ）在生产过程中需用乙醇进行多次重结晶精制，故原料药中残留乙醇，这不仅影响药物的药效，而且可能影响药物的稳定性。药物中残留有机溶剂...     

Diethylene glycol monomethyl ether, ethylene glycol monomethyl ether and the metabolite, 2-methoxyacetic acid affect in vitro chondrogenesis

Diethylene glycol monomethyl ether (DEGME), ethylene glycol monomethyl ether (EGME) and their common metabolite, methoxyacetic acid (MAA) have been associated with adverse reproductive effects. The objective of this research is to investigate the effects of DEGME, EGME and MAA on in vitro chondrogenesis and the mechanisms by which these effects occur. Micromass cultures were exposed to DEGME, EGME or MAA for 5 days and proteoglycan abundance and cell proliferation determined. Longer-term 9- and 14-day cultures were exposed to MAA and apoptosis analyzed. All three chemicals decreased proteoglycan abundance and cell proliferation at the highest dose tested (100 μL/mL). However, only MAA showed a dose-dependent effect for both parameters at 0.01, 10, and 100 μL/mL. Furthermore, micromass cultures show an increase in apoptotic cells which when treated with MAA suggest that cell death could result from induced apoptosis. These results suggest that effects of DEGME and EGME are the result of generalized toxicity, but their metabolite MAA induces mitochondrial-mediated apoptosis during in vitro chondrogenesis.     

Hydrolysis kinetics of propylene glycol monomethyl ether acetate in rats in vivo and in rat and human tissues in vitro.

The kinetic equivalency of propylene glycol monomethyl ether (PGME), derived from propylene glycol monomethyl ether acetate (PGMEA), as well as the parent compound (PGME) following intravenous administration to Fischer 344 rats was evaluated. In addition, in vitro hydrolysis rates of PGMEA in blood and liver tissue from rats and humans were determined. The blood kinetics were determined following iv administration to rats of PGME and PGMEA of low [10 and 14.7 mg/kg body weight (bw)] or high (100 and 147 mg/kg) equimolar dosages of PGME and PGMEA, respectively. The blood time courses of PGME elimination for both dosages of both compounds were identical. Half-lives of PGMEA elimination following iv administration of 14.7 or 147 mg PGMEA/kg bw were calculated to be 1.6 and 2.3 min, respectively. Rat and human in vitro hydrolysis rates of PGMEA were determined by incubation of 5 or 50 microg PGMEA/ml in whole blood or liver homogenate. The rate of loss of PGMEA was more rapid in rat blood than in human blood, with hydrolysis half-lives of 36 and 34 min in human blood and 16 and 15 min in rat blood for the 5 and 50 microg/ml concentrations of PGMEA, respectively. In contrast the rate of loss of PGMEA in human and rat liver homogenate incubations was similar, 27-30 min and 34 min, respectively. These data demonstrate the rapid hydrolysis of PGMEA in vivo to its parent glycol ether, PGME and that, once hydrolyzed, the kinetics for PGME derived from PGMEA are identical to that for PGME. This study supports the use of the toxicological database on PGME as a surrogate for PGMEA.     

Electrophoresis of phosphoglycerate kinase-2 to determine testicular damage induced by ethylene glycol monomethyl ether and sterility associated with chromosomal abnormality

Phosphoglycerate kinase (PGK, EC 2.7.2.3), which is expressed specifically in sperm and spermatids, is an enzyme in the Embden-Meyerhof pathway that converts glucose to pyruvate. We developed an electrophoresis method to determine relative PGK-2 quantity and applied it to evaluate spermatogenesis activity. In the ethylene glycol monomethyl ether (EGME)-induced testicular toxicity, relative PGK-2 quantity had not decreased until 4 weeks of exposure. Mean relative PGK-2 quantities, defined as PGK-2 quantity over PGK-1 quantity in a pooled spleen sample (±SD) were: 1.43±0.32 for control animals (N=10); 1.67±0.24 for the group exposed at 500 mg/kg for 5 days (N=6); 1.85±0.58 for the group exposed at 500 mg/kg for 2 weeks (N=6); 0.09±0.06 for the group exposed at 500 mg/kg for 4 weeks (N=6); not detectable in animals exposed at 500 mg/kg for 5 weeks (N=7); 0.208±0.103 for the group exposed at 250 mg/kg for 5 weeks (N=6); and 1.35±0.38 for the group exposed at 125 mg/kg for 5 weeks (N=6). These relative quantities showed a good correlation with sperm/spermatid counts (r=0.823,p<0.01) and histological findings. These findings suggest that EGME has toxicity on primary spermatocytes and spermatogonia. In the case of sterility associated with a chromosomal abnormality (chromosomal translocation between chromosome X and 16), relative PGK-2 quantity was not detected in any of the seven adult (12 weeks of age) mice, although many primary spermatocytes were detected by histological examination. Those findings suggest that cellular differentiation is arrested at meiosis due to the chromosomal abnormality. It was thus concluded that relative PGK-2 quantity provides information on testicular development and is therefore useful as an indicator of testicular function.     

Effects of sulpiride and ethylene glycol monomethyl ether on endometrial carcinogenicity in Donryu rats

Sulpiride and ethylene glycol monomethyl ether (EGME) are known ovarian toxicants that stimulate prolactin (PRL) secretion, resulting in hypertrophy of the corpora lutea and increased progesterone (P4) production. The purpose of the present study was to investigate how the PRL stimulatory agents affected uterine carcinogenesis and to clarify the effects of PRL on endometrial adenocarcinoma progression in rats. Ten‐week‐old female Donryu rats were treated once with N‐ethyl‐N′‐nitro‐N‐nitrosoguanidine (20 mg kg^?1), followed by treatment with sulpiride (200 ppm) or EGME (1250 ppm) from 11 weeks of age to 12 months of age. Sulpiride treatment inhibited the incidence of uterine adenocarcinoma and precancerous lesions of atypical endometrial hyperplasia, whereas EGME had no effect on uterine carcinogenesis. Sulpiride markedly prevented the onset of persistent estrus throughout the study period, and EGME delayed and inhibited the onset of persistent estrus. Moreover, sulpiride‐treated animals showed high PRL and P4 serum levels without changes in the levels of estradiol‐17β, low uterine weights and histological luteal cell hypertrophy. EGME did not affect serum PRL and P4 levels. These results suggest that the prolonged low estradiol‐17β to P4 ratio accompanied by persistent estrous cycle abnormalities secondary to the luteal stimulatory effects of PRL may explain the inhibitory effects of sulpiride on uterine carcinogenesis in rats. Copyright © 2015 John Wiley & Sons, Ltd.     

乙基纤维素膜中壬苯醇醚的释放

目的考察水不溶高分子乙基纤维素薄膜中具有两亲性质的壬苯醇醚的释放行为,考察水微溶阳离子表面活性剂三甲基十六烷基溴化铵的添加对壬苯醇醚释放的影响。方法以刮板法制备5种乙基纤维素载药薄膜,使壬苯醇醚载药量与乙基纤维素质量比为1.5∶10.0、5.0∶10.0、10.0∶10.0、20.0∶10.0、40.0∶10.0,同样以刮板法制备6种添加有三甲基十六烷基溴化铵的薄膜,使壬苯醇醚,三甲基十六烷基溴化铵与乙基纤维素质量比1.5∶0.5∶10.0、1.5∶1.0∶10.0、5.0∶0.5∶10.0、5.0∶1.0∶10.0、10.0∶0.5∶10.0、10.0∶1.0∶10.0。以去离子水为释放介质,37℃,120 r.min-1条件下考察药物的释放,采用HPLC法测定释放介质中药物的量,绘制8 h内的药物累计释放曲线并进行拟合。结果乙基纤维素薄膜中壬苯醇醚载药量的高低,可以使得其8 h内的释放行为从没有释放到30 min内完全突释,2个系列的样品具有缓释能力,并且载药量越大同一时间点乙基纤维素薄膜中壬苯醇醚的释放量越大。添加三甲基十六烷基溴化铵能促进壬苯醇醚的释放。具有缓释行为的样品的释药曲线对Higuchi's和1级释放方程拟合均较好。结论在乙基纤维素薄膜中,壬苯醇醚的载药量可以影响其自身的释放行为,三甲基十六烷基溴化铵的添加和增多可加速壬苯醇醚的释放,为研究其它类型乙基纤维素/壬苯醇醚共混系统药物释放行为提供了参考。     

Differential gene expression detected by suppression subtractive hybridization in the ethylene glycol monomethyl ether-induced testicular lesion.

The solvent ethylene glycol monomethyl ether (EGME) produces the same testicular lesions in rodents and human testis cultures, whose onset is characterized by apoptosis of pachytene spermatocytes. To identify gene changes early in the lesion and determine the possible involvement of cells other than the spermatocytes, we employed a suppression subtractive hybridization technique using whole testes from mice treated 8 h previously with 500 mg/kg EGME to generate two subtracted mouse testis cDNA libraries enriched for gene populations either up-regulated or down-regulated by EGME. A total of 70 clones were screened, and 6 of them were shown by Northern blotting to be differentially expressed in the EGME lesion. The three clones with increased expression after EGME treatment were identical to t-complex testis expressed gene 1 (tctex1), a gene encoding ribosomal protein S25, and a heretofore uncharacterized mouse testis expressed sequence tag. Three other genes suppressed by EGME were tctex2, alpha-2,6-sialyltransferase gene, and another uncharacterized mouse testis expressed sequence tag. Predicted peptide sequences of these clones contain multiple motifs for phosphorylation, glycosylation, and myristoylation. In situ hybridization with the antisense RNA probes further supported the expression changes of these six clones and localized the changes in multiple germ cell stages as well as other cell types (Sertoli, interstitial and peritubular cells). These data at the gene expression level are the first to demonstrate the early involvement in this lesion of cell types other than the dying spermatocytes.     

药物中石油醚残留量的气相色谱检测方法学探讨

目的:采用气相色谱法对药物中残留的石油醚进行定量检测方法学探讨。方法:以市售石油醚(60～90℃)为例,结合新药尼非韦罗中涉及的甲醇、乙醇、二氯甲烷、乙酸乙酯、四氢呋喃以及1,4-二氧六环的分离情况,建立气相色谱条什。在分析了石油醚(60～90℃)的组分分布基础上,对其定量测定办法分别探讨了了单一组分的峰面积计算方式和主成分(按信噪比大于10)峰面积加和方式。结果:发现石油醚(60～90℃)在药物中的残留量计算采用主成分峰面积加和方式较合理,而且石油醚(60～90℃)和上述6种有机溶剂在相应的检测范围内线性良好,回收率均令人满意。结论:石油醚(60～90℃)在药物中的残留定量计算方式采用主成分峰面积加和法可以减少由于不同厂家来源或者不同批号的石油醚组分比例差异导致的汁算偏差,从而可以较好地满足对相关药物的质量控制要求。     

Toxicity Review of Ethylene Glycol Monomethyl Ether and its Acetate Ester

Ethylene glycol monomethyl ether (EGME) and its acetate ester (EGMEA) are highly flammable, colorless, moderately volatile liquids with very good solubility properties. They are used in paints, lacquers, stains, inks and surface coatings, silk-screen printing, photographic and photo lithographic processes, for example, in the semiconductor industry, textile and leather finishing, production of food-contact plastics, and as an antiicing additive in hydraulic fluids and jet fuel.

EGME and EGMEA are efficiently absorbed by inhalation as well as via dermal penetration. Dermal absorption may contribute substantially to the total uptake following skin contact with liquids or vapours containing EGME or EGMEA. EGMEA is rapidly converted to EGME in the body and the two substances are equally toxic in animals. Therefore, the two substances should be considered as equally hazardous to man.

Effects on peripheral blood, testes, and sperm have been reported at occupational exposure levels ranging between 0.4 and 10?ppm EGME in air, and with additional, possibly substantial, dermal exposure. Severe malformations and disturbed hematopoiesis have been linked with exposure to EGME and EGMEA at unknown, probably high, levels. Embryonic deaths in monkeys and impaired spermatogenesis in rabbits have been reported after daily oral doses of 12 and 25?mg per kg body weight, respectively. In several studies, increased frequency of spontaneous abortions, disturbed menstrual cycle, and subfertility have been demonstrated in women working in the semiconductor industry. The contribution of EGME in relation to other exposure factors in the semiconductor industry is unclear.     

顶空毛细管气相色谱法测定硝酸异康唑中5种有机溶剂残留

目的:建立测定硝酸异康唑原料药中甲基叔丁基醚、甲醇、二氯甲烷、三氯甲烷、四氢呋喃5种有机溶剂残留量的分析方法。方法:采用毛细管气相色谱法,检测器:FID;检测器温度:250℃;进样器温度:200℃;载气:氮气;顶空进样。结果:在上述色谱条件下,甲基叔丁基醚、四氢呋喃、甲醇、二氯甲烷和三氯甲烷分别在10.28~92.52μg·mL^-1 (γ=0.9994),14.49~130.43μg·mL^-1 (γ=0.9994),62.86~565.74μg·mL^-1 (γ=0.9993),13.52~121.68μg·mL^-1 (γ=0.9995),2.76~24.84μg·mL^-1 (γ=0.9991)质量浓度范围内线性关系良好。平均回收率分别为97.19% (RSD为1.21%),99.90% (RSD为0.28%),99.29% (RSD为1.21%),99.15% (RSD为0.65%),100.14% (RSD为2.58%)。结论:该检测方法灵敏、准确、可靠,可用于硝酸异康唑原料药的质量控制。