顶空气相色谱法同时测定黄蜀葵花总黄酮提取物中9种有机溶剂的残留量

Simultaneous Determination of 9 Kinds of Organic Solvents Residues in Total Flavonoids Extracts from Abelmoschus manihot by Headspace GC

目的:建立同时测定黄蜀葵花总黄酮提取物中9种有机溶剂残留量的方法。方法:采用顶空气相色谱法测定黄蜀葵花总黄酮提取物中苯、丙烯腈、甲基丙烯酸甲酯、甲苯、1,2-二氯乙烷、二甲苯、氯苯、苯乙烯、二乙烯苯等9种残留溶剂的含量。色谱柱为AgilentDB-WAX毛细管柱(30m×0.25mm,0.25μm),程序升温;氢焰离子化检测器温度为250℃,进样口温度为250℃;载气为氮气,流速为1.2mL/min,分流比为10∶1;顶空进样量为1mL,顶空平衡温度为90℃,平衡时间为45min。结果:9种待测成分色谱峰之间的分离度均大于1.5,空白溶剂(10%N-甲基吡咯烷酮水溶液)无干扰;其检测质量浓度的线性范围分别为0.16~1.21、0.80~6.03、1.61~12.09、1.62~12.12、0.16~1.21、1.60~12.01、0.81~6.11、1.60~12.03、0.80~6.03 μg/mL(r≥0.999 4);定量限分别为0.162 08、0.201 08、0.080 6、0.080 768、0.161 92、0.400 36、0.040 712、0.026 736、0.013 395μg/mL,检测限分别为0.040 52、0.040 216、0.026 87、0.026 9、0.040 48、0.080 072、0.013 57、0.008 912、0.004 465 μg/mL;精密度试验(n=5)、重复性试验(n=6)的RSD均小于5%;平均回收率为99.41%~111.27%(RSD<9%,n=9)。3批黄蜀葵花总黄酮提取物中试样品中均未检出上述9种残留溶剂。结论:所建立方法简便、准确、可靠,可用于黄蜀葵花总黄酮提取物中9种有机溶剂残留量的同时测定。

OBJECTIVE:To establish a method for simultaneous determination of 9 kinds of organic solvents residues in total flavonoids extracts from Abelmoschus manihot. METHODS:Headspace GC was adopted to determine the contents of 9 kinds of organic solvents residues in total flavonoids extracts from A. manihot,such as benzene,acrylonitrile,methyl methacrylate, toluene,1,2-dichloroethane,xylene,chlorobenzene,styrene and divinylbenzene. The determination was performed on Agilent DB-WAX capillary column(30 m×0.25 mm,0.25 μm)through temperature-programmed route. The inlet temperature and FID detector temperature were set at 250 ℃. The carrier gas was nitrogen with the flow rate of 1.2 mL/min. The split ratio was 10 ∶ 1. The containers of headspace injector were in equilibrium at 90 ℃ for 45 min and the sample size was 1 mL. RESULTS:The separation degree among the peaks of 9 components was greater than 1.5,and the blank solvent (10% N-methyl pyrrolidone aqueous solution)had no interference. The linear ranges of them were 0.16-1.21,0.80-6.03,1.61-12.09,1.62-12.12,0.16-1.21, 1.60-12.01,0.81-6.11,1.60-12.03,0.80-6.03 μg/mL,respectively(r≥0.999 4). The limits of quantitation were 0.162 08,0.201 08, 0.080 6,0.080 768,0.161 92,0.400 36,0.040 712,0.026 736,0.013 395 μg/mL;the limits of detection were 0.040 52,0.040 216, 0.026 87,0.026 9,0.040 48,0.080 072,0.013 57,0.008 912,0.004 465 μg/mL,respectively. RSDs of precision(n=5)and reproducibility(n=6)tests were all lower than 5%. Average recoveries were 99.41%-111.27%(RSD<9%,n=9). Above 9 residual solvents were not detected in 3 batches of total flavonoids extracts from A. manihot. CONCLUSIONS:Established method is simple,accurate and reliable,and can be applied for simultaneous detection of 9 kinds of organic solvents residues in total flavonoids extracts from A. manihot.