气相色谱法检查依托咪酯注射液中二甘醇的含量

目的建立依托咪酯注射液中二甘醇检查方法。方法采用气相色谱法,以丙三醇为内标,色谱柱为INNOWAX毛细管柱（30m×0.53mm×1μm）,汽化室温度220℃,程序升温：初始温度为120℃,保持3分钟;以每分钟10℃的速度升至230℃,保持5min。载气：氮气,4mL·min^-1;检测室温度250℃,尾吹30mL·min^-1,进样量1μL。结果上述测定方法能使内标（丙三醇）、1,2-丙二醇、1,3-丙二醇和二甘醇良好分离,在11μg·mL^-1-167μg·mL^-1的范围内浓度（C）与峰面积响应值（f=A/A内）有良好的线性关系,r=0.9995;进样精密度、日内测定精密度、日间测定精密度的RSD%分别为1.1%、0.9%和1.0%;平均回收率（n=9）为100.9%,RSD为1.5%;方法定量限和检测限分别为0.56μg·mL^-1,0.17μg·mL^-1。结论气相色谱法可以用于检查控制依托咪酯注射液中二甘醇的含量。     

气相色谱法测定药物中二甘醇的含量

目的采用气相色谱法测定药物中二甘醇的含量。方法采用键合6%氰丙基-96%二甲基聚硅氧烷毛细管柱（DB-624）,程序升温：初始100℃,以7.5℃.min^-1升至220℃,保持4 min。气化室温度：240℃;FID检测器温度：250℃;载气：氮气。结果二甘醇线性范围为0.05-0.5 mg.mL^-1（r=0.999 5）;平均回收率为99.4%（RSD=1.2%;n=9）。结论本法准确、简便,适用于测定药物中二甘醇的含量。     

GC法测定聚山梨酯65/85中乙二醇、二甘醇、三甘醇及环氧乙烷和二氧六环杂质的含量

目的:建立新型药用辅料聚山梨酯65/85中乙二醇、二甘醇和三甘醇以及环氧乙烷和二氧六环杂质的检查方法。方法:乙二醇、二甘醇和三甘醇的检测为气相色谱直接进样法;环氧乙烷和二氧六环的检测为顶空气相色谱法。2种检查方法均为氢火焰离子化检测器(FID)。结果:乙二醇、二甘醇和三甘醇分别在5.10～101.92、5.06～101.28、5.00～100.04μg·mL^-1的浓度范围内线性关系良好(r_乙二醇=1.000;r_二甘醇=0.999 9;r_三甘醇=0.999 8);检测限分别为0.27、0.25、0.29μg·mL^-1;定量限分别为0.55、0.50、1.15μg·mL^-1;重复性RSD均<5%;回收率在91.3%～97.3%。环氧乙烷和二氧六环分别在1.00～10.00、0.50～40.00μg·mL^-1浓度范围内线性关系良好(r_环氧乙烷=0.999 8;r_二氧六环=0.999 9);检...     

气相色谱法测定依托泊苷注射液中乙二醇与二甘醇的量

目的采用气相色谱（GC）法测定依托泊苷注射液中乙二醇与二甘醇的量。方法色谱柱为DB-WAXetr毛细管柱（30m×0.32mm,1.0μm）,采用程序升温方式。结果乙二醇检测质量浓度在1.60～667.8μg/mL范围内与峰面积线性关系良好,线性回归方程为Y=523.59X-2.8439（r=0.9998）,平均回收率为103.1%,RSD为1.9%（n=9）;二甘醇检测质量浓度在1.61～670.2μg/mL范围内与峰面积线性关系良好,线性回归方程为Y=567.48X-1.8425（r=0.9999）,平均回收率为99.8%,RSD为1.6%（n=9）。结论 GC法简单、灵敏,可用于依托泊苷注射液的质量控制。     

气相色谱法测定聚山梨酯80中二甘醇的含量

目的建立一种气相色谱法测定聚山梨酯80中二甘醇的含量.方法色谱柱:以聚乙二醇(PEG-20M)为固定液的极性毛细管柱(30m×0.32mm,0.50μm);检测器:氢火焰离子检测器(FID);检测器温度230℃;进样口温度200℃;柱温度:程序升温,初始温度60℃,保持3min,再以10℃·min-1升温至230℃保持10min;载气:高纯氮气.结果二甘醇线性范围为0.025～0.25mg·mL-1(r=0.9993);平均回收率101.57%(RSD=1.505%,n=5).结论本方法简单、结果准确、重现性好,可用于聚山梨酯80中二甘醇含量的测定.     

毛细管气相色谱法测定聚桂醇原料中乙二醇、月桂醇、二甘醇的含量

目的:建立聚桂醇原料药中3个有关物质乙二醇、月桂醇和二甘醇的毛细管气相色谱测定方法。方法:采用DB-WAX(30 m×0.32 mm×0.25μm)毛细柱,氢火焰离子检测器(FID),进样口温度230℃,检测器温度250℃,程序升温(起始温度180℃,维持7 min,以15℃.min-1的速率升温至230℃,维持40 min)。结果:在选定的色谱条件下,3个物质分离良好。乙二醇的回归方程为Y=846.8X-1.830(r=0.9993),线性范围为0.004～0.2 mg·mL-1,平均回收率为100.0%(n=9);月桂醇的回归方程为Y=2.694×103X-121.8(r=0.9992),线性范围为0.08～4.0 mg·mL-1,平均回收率为100.7%(n=9);二甘醇的回归方程为Y=1.018×103X-3.010(r=0.9992),线性范围为0.004～0.2 mg·mL-1,平均回收率为99.6%(n=9)。结论:本方法能用于聚桂醇原料的质量检测。     

丙二醇质量控制方法和二甘醇检查方法探讨

目的对丙二醇质量控制方法和二甘醇检查方法进行理论探讨和实践研究。方法在对丙二醇和二甘醇进行简要介绍的基础上,通过分析《中国药典（2005年版,二部）》对丙二醇质量控制方法,指出目前药典方法存在的不足,并通过实验研究提出解决方案。结果药典规定的质量控制方法不能完全保证丙二醇的质量,新的质量控制方法应包括丙二醇的含量测定和二甘醇检查。结论GC—MS法可作为丙二醇含量测定和二甘醇检查的参考方法。     

GC—MS法应用于丙二醇的质量控制及二甘醇检查

目的：建立丙二醇的质量控制和二甘醇检查的方法。方法：应用气相色谱-质谱联用仪（GC—MS）对丙二醇和二甘醇同时进行分析；色谱柱起始温度40℃，维持时间5min，以20℃&#183;min^-1速率升至80℃，维持1min．再以30℃&#183;min^-1升至250℃，维持5min，不分流进样，通过监测总离子流色谱图以及色谱峰的质谱图，对丙二醇、杂质以及二甘醇进行检测。结果：该方法对丙二醇和二甘醇都具有良好的专属性、灵敏度和精密度。结论：该方法能用于丙二醇的质量控制和其中的二甘醇的检查。     

高效液相色谱法检测发酵液中二羟基丙酮和甘油的含量

目的建立二羟基丙酮(DHA)发酵过程中产物和残余甘油底物的高效液相色谱检测方法。方法流动相为乙腈-水(90:10),色谱柱为Lichrospher 5-NH2(4.6 mm×250 mm),用紫外检测器在271 nm处检测DHA,用示差折光检测器检测甘油。结果DHA的线性范围为2.00~12.00 mg/mL,最低检出限(LOD)和最低定量限(LOQ)分别为0.30和1.20 mg/mL。甘油的线性范围为1.00~10.00 mg/mL,LOD和LOQ分别为0.22和0.50 mg/mL。结论此文建立的DHA和甘油的检测方法精密度好,准确性高,不受发酵液中其他杂质的影响,可以应用于DHA发酵过程中底物和产物的检测。     

气相色谱法测定甘油乙醇洗手液中甘油和乙醇含量

目的建立同时测定甘油乙醇洗手液中甘油乙醇含量的气相色谱法。方法采用直接进样法。色谱柱为HP-Innowa毛细管柱(30 m×0.53 mm,1.0μm),载气为氮气;氢火焰离子化检测器,进样口温度为350℃,检测器温度为380℃;柱温起始温度为100℃,维持3 min,以100℃/min的速率升温至240℃,维持7 min。结果乙醇、甘油的检测质量浓度线性范围分别是0.12～0.36 g/mL(r=0.999 6)和0.007 6～0.022 8 g/mL(r=0.999 2)。结论该方法准确、可靠,可同时有效测定甘油乙醇洗手液中甘油和乙醇含量。     

开塞露(含甘油)含量测定方法的改进

目的：对开塞露(含甘油)含量测定方法进行改进。方法：改变样品的取样量,按国家药品标准WS₁-XG-018-2011对不同厂家的开塞露(含甘油)进行含量测定。结果：样品的取样量在0.10g~0.19g之间,反应完全,滴定结果准确,重现性好。结论：改进方法后,能更准确的测定甘油的含量,建议修改原标准。     

Diethylene Glycol in Health Products Sold Over-the-Counter and Imported from Asian Countries

Diethylene glycol (DEG), a chemical that has been implicated in multiple medication-associated mass poisonings, can result in renal and neurological toxicity if ingested. Three previous such mass poisonings implicated Chinese manufacturers as the origin of contaminated ingredients. No literature exists on potential DEG or triethylene glycol (TEG), a related compound, contamination of health products imported from Asian countries to the USA. Our primary objective was to quantitatively assess the amount of DEG present in a convenience sampling of these health products. The study’s secondary objectives were to: (1) evaluate for, and quantify TEG levels in these samples; (2) compare DEG and TEG levels in these products directly to levels in medications implicated in previous similar mass poisonings; and (3) to estimate DEG dose (in mg/kg) based on the manufacturer’s instructions and compare these values to toxic doses from past mass poisonings and the literature. A quantitative assessment of DEG and TEG was performed in a convenience sampling of over-the-counter health products imported from Asian countries. Results were converted to volume to volume (v/v) % and compared with DEG levels in medications implicated in previous mass poisonings. Estimated doses (based on the manufacturer’s instructions) of each product with detectable levels of DEG for a 70 kg adult were compared to toxic doses of DEG reported in the literature. Seventeen of 85 (20%) samples were not able to be analyzed for DEG or TEG due to technical reasons. Fifteen of 68 (22%) samples successfully tested had detectable levels of DEG (mean, 18.8 μg/ml; range, 0.791–110.1 μg/ml; and volume to volume (v/v) range, 0.00007–0.01%). Two of 68 (3%) samples had TEG levels of 12.8 and 20.2 μg/ml or 0.0012% and 0.0018% TEG v/v. The product with the highest DEG% by v/v was 810 times less than the product involved in the Panama DEG mass poisoning (8.1%). The lowest reported toxic dose from a past DEG mass poisoning (14 mg/kg) was more than 150 times higher than the highest daily dose estimated in our study (0.09 mg/kg). Sixty-eight of 85 (80%) samples were able to be successfully analyzed for DEG and TEG. DEG and TEG were detectable in 15/68 (22%) and 2/68 (3%) samples, respectively. Based on current standards, these levels probably do not represent an acute public health threat. Additional research focusing on why DEG is found in these products and on the minimum amount of DEG needed to result in toxicity is needed.     

GC法测定葛根素注射液中丙二醇和二甘醇的残留量

采用气相色谱法测定葛根素注射液中丙二醇和二甘醇的残留量.用DB-WAXetr毛细管柱,检测器温度为280℃.丙二醇的测定在49.69～993.8цg·mL-1范围内线性关系良好,平均回收率为98.4%,RSD=1.2%(n=9);二甘醇在11.09～110.9цg·mL-1范围内线性关系良好,平均回收率为99.2%,RSD=1.4%(n=9).方法简单、灵敏度高.     

气相色谱法测定羟乙基淀粉中乙二醇的残留量

建立GC法测定羟乙基淀粉中乙二醇的残留量。羟乙基淀粉中残留的乙二醇,通过与六甲基二硅氮烷的衍生化反应生成三甲基硅烷衍生物,再用气相色谱法进行测定。乙二醇在1.5~50μg.mL-1浓度范围内线性关系良好,相关系数r=0.9992,平均回收率为99.6%(n=5),RSD为1.2%,最低检测限为0.6 ng。本法灵敏度高,简便易行,结果准确可靠。     

Screening method for ethylene glycol and diethylene glycol in glycerin-containing products

This paper describes a capillary gas chromatographic method with flame ionization detection for the identification/quantification of ethylene glycol (EG) and diethylene glycol (DEG) in glycerin. The validation study shows that the proposed method is specific, sensitive, precise, and accurate. The linear range of the method was 0.013–0.031 mg/mL for EG and 0.012–0.030 mg/mL for DEG. Wider ranges may be achievable but were not investigated. The limit of detection of EG and DEG were determined as 0.0018% and 0.0036% (w/w) respectively, and at this concentration the signal-to-noise ratios for EG and DEG were approximately 3:1. The method was also used to determine EG and DEG in toothpaste. The results were compared to those obtained by thin-layer chromatography (TLC) and showed greater sensitivity and specificity.     

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.