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气相色谱法测定头孢匹胺中的残留溶剂
【摘要】 目的 建立测定头孢匹胺中的残留溶剂含量的方法。方法 采用气相色谱法，用涂渍PEG�20M的填充柱,N2为载气，柱温100 ℃，以正丁醇为内标物，FID检测。结果 丙酮、乙腈和二甲基甲酰胺分别在进样量0.500～2.000 μg、0.041～0.164 μg和0.088～0.352 μg范围内, 与相应溶剂峰/内标峰的面积比值线性关系良好(r分别为0.9997、0.9994和0.9999), 丙酮、乙腈和二甲基甲酰胺的平均回收率分别为101.0%、97.7%和100.4%，重复进样峰面积RSD分别为0.31%、1.28%和0.73%（n=5）。结论 所建立的方法专属性好，简便准确，可用于检测头孢匹胺中的残留溶剂。
【关键词】 气相色谱法 头孢匹胺 残留溶剂 丙酮 乙腈 二甲基甲酰胺
Abstract:Objective To establish a method for content determination of the residual solvents in cefpiramide. Methods The analysis was performed on a column coated by PEG�20M under the column temperature of 100 ℃, with N2 as carrier gas. Results The standard curves of acetone, acetonitrile and N,N�dimethylformamide were linear within the ranges of 0.500～2.000 μg, 0.041～0.164 μg and 0.088～0.352 μg(r=0.9997, 0.9994 and 0.9999), respectively. The average recoveries of acetone, acetonitrile and N,N�dimethylformamide were 101.1%, 97.7% and 100.4%, while the RSD for replications were 0.31%,1.28% and 0.73%（n=5）,respectively. Conclusion The method is specific, simple and accurate for the quality control cefpiramide raw materials.
Key words: GC; cefpiramide; residual solvent; acetone; acetonitril; N,N�dimethylformamide
头孢匹胺（cefpiramide）是第三代头孢菌素类广谱抗生素，可进一步加工成钠盐或直接用于临床,对革兰氏阳性菌、阴性菌及厌氧菌均有强大的抗菌活力，对β�内酰胺酶稳定性好，有良好的临床价值〔1〕。由于各厂生产的头孢匹胺采用工艺和使用的溶剂不同，因而残留溶剂的种类也有所不同，需分别研究出适合的方法进行准确测定。本研究基于广州白云山化学制药厂生产的头孢匹胺产品，其生产过程中使用到国际协调组织（ICH）规定的二类溶剂乙腈和二甲基甲酰胺，以及三类溶剂丙酮,应在质量标准中加以监控。已有文献〔2-3〕报道类似品种头孢匹胺钠中残留溶剂的测定方法，但由于被测残留溶剂种类不同而不可直接引用。本文报道的气相色谱法，专属性强，能在同一次试验中同时测定3种溶剂的含量，无需程序升温，方法简便准确。
1 仪器与试药
岛津GC�14A气相色谱仪；大连依利特公司产的涂渍PEG�20M的填充玻璃柱（3.2 mm×2 m）。丙酮和二甲基甲酰胺对照品（均为分析纯试剂，含量100.0%），乙腈对照品（为色谱纯试剂，含量100.0%），头孢匹胺原料由广州白云山化学制药厂提供，高纯度氮气由广州气体厂生产。
2 方法与结果
2.1 色谱条件与测定法
用涂渍PEG�20M的填充玻璃柱，以氮气为载气，流量10 mL/min,进样口温度210 ℃，柱温100 ℃，氢火焰离子化检测器温度250 ℃。
称取正丁醇适量，加水制成50 μg/mL的溶液，作为内标液。精密称取丙酮对照品约100 mg、乙腈对照品约8 mg和二甲基甲酰胺对照品约18 mg置100 mL量瓶中，加内标液溶解并稀释至刻度，摇匀，作为对照品溶液。精密称取头孢匹胺供试品约1 g，置具塞试管中，准确加入内标液5 mL，强力振摇5 min，过滤，取续滤液作为供试品溶液。分别精密量取对照品溶液和供试品溶液1 μL，注入气相色谱仪，记录色谱图，用内标法以峰面积计算。
2.2 色谱参数、检测限和定量限
头孢匹胺供试品溶液的色谱图见图1，丙酮、乙腈、正丁醇（内标）和二甲基甲酰胺峰柱效分别为850、800、600和1 000，拖尾系数分别为1.4、1.2、1.3和1.3, 丙酮与乙腈、乙腈与正丁醇及正丁醇与二甲基甲酰胺峰之间分离度分别为3.9、2.8和7.7。丙酮、乙腈和二甲基甲酰胺的检测限（信噪比3∶1）分别为1 ng、0.5 ng和0.5 ng,定量限（信噪比10∶1）分别为2 ng、1 ng和2 ng。
a.丙酮;b.乙腈;c.正丁醇;d.二甲基甲酰胺
图1 头孢匹胺中的残留溶剂气相色谱图（略）
Fig.1 GC Chromatograms of the residual solvents in the raw materials
2.3 精密度试验
取对照品溶液重复进样5次，测得丙酮、乙腈和二甲基甲酰胺峰面积与内标峰面积比的RSD分别为0.31%、1.28%和0.73%。同一份均匀样品，在不同仪器、不同操作者条件下测得3份结果，算出丙酮、乙腈和二甲基甲酰胺含量结果重现性分别为1.5%、1.9%和1.7%。
2.4 线性关系与范围
分别精密称取丙酮、乙腈和二甲基甲酰胺对照品, 按“2.1”项方法分别用内标溶液定量配制并稀释成质量浓度分别为丙酮500、750、1 000、1 500 μg/mL，乙腈41、61.5、82、123、164 μg/mL和二甲基甲酰胺88、132、176、264、352 μg/mL的溶液，各准确进样1 μL测定，结果进样量（m)与待测溶剂峰面积/内标峰面积比值（A）的线性回归方程分别为：丙酮 A1=9.4826m1-0.2456（r=0.9997）,乙腈 A2=13.4495m2+0.03646（r=0.9994）,二甲基甲酰胺 A3=4.3421m3+0.0094（r=0.9999）；丙酮、乙腈和二甲基甲酰胺的进样量测定范围分别为0.500～2.000 μg、0.041～0.164 μg和0.088～0.352 μg。
2.5 回收率试验
按“2.1”项方法, 分别用内标液配制对照品溶液,供试品溶液，以及丙酮、乙腈和二甲基甲酰胺的浓度均相当于对照品溶液的80%、100%和120%的供试品加对照品溶液各3份, 依法进样测定, 算出丙酮、乙腈和二甲基甲酰胺的加样回收结果如下：
丙酮：100.1%、104.6%、100.5%、101.4%、102.9%、99.3%、100.0%、99.3%和100.8%，平均101.0%（RSD 1.75%）。
乙腈：97.1%、97.5%、96.1%、99.8%、96.6%、96.3%、99.0%、99.2%和97.9%，平均97.7%（RSD 1.40%）。
二甲基甲酰胺:101.2%、99.3%、100.8%、102.8%、101.4%、99.6%、99.3%、98.6%和101.0%，平均100.4%（RSD 1.32%）。
2.6 样品测定
按“2.1”项方法分别测定头孢匹胺样品3批，测得其丙酮含量分别为：0.015%、0.013%和0.011%；乙腈含量分别为0.013%、0.011%和0.010%；二甲基甲酰胺含量分别为0.005%、0.002%、0.001%,均符合ICH建议的限度（0.5%、0.041%和0.088%）。
3 讨论
3.1 3种溶剂均有很好的水溶性，头孢匹胺样品加水强力振摇后形成极细微颗粒的混悬液，能保证残留溶剂的溶出。
3.2 二甲基甲酰胺为较高沸点的溶剂，其水溶液难以采用顶空进样法测定，且二甲基甲酰胺直接进样对毛细管柱伤害较大，因而选用填充柱直接进样法。
3.3 本试验采用恒定柱温条件下测定有利于测定稳定性，采用内标法有利于减少进样操作的误差。
3.4 以上试验表明，本气相色谱法专属性强，能在恒定柱温条件下同时测定3种残留溶剂的含量，方法快捷准确，可用于头孢匹胺残留溶剂的监控。
【参考文献】
〔1〕 周乐，王明贵.头孢匹胺的体外抗菌作用〔J〕.中国抗生素杂志，1997，22（4）：275-278.
〔2〕 王喜梅，李晓燕，周海云，等.顶空法测定头孢匹胺钠中的溶剂残留〔J〕.中山大学学报：自然科学版，2004，43（4）：122-124.
〔3〕 李弘韬，杨敏，万江陵，等.顶空固相微萃取-气相色谱法测定头孢匹胺钠中多种有机溶剂残留量〔J〕.药物分析杂志，2005,25（1）：37-39.
〔4〕 国家药典委员会.中华人民共和国药典：二部〔S〕.北京：化学工业出版社，2005：附录V E和附录VIII P.
Gas chromatography cefpiramide of Residual Solvents
Abstract:Objective To establish a method for content determination of the residual solvents in cefpiramide. Methods The analysis was performed on a column coated by PEG�20M under the column temperature of 100 ℃, with N2 as carrier gas. Results The standard curves of acetone, acetonitrile and N,N�dimethylformamide were linear within the ranges of 0.500～2.000 μg, 0.041～0.164 μg and 0.088～0.352 μg(r=0.9997, 0.9994 and 0.9999), respectively. The average recoveries of acetone, acetonitrile and N,N�dimethylformamide were 101.1%, 97.7% and 100.4%, while the RSD for replications were 0.31%,1.28% and 0.73%（n=5）,respectively. Conclusion The method is specific, simple and accurate for the quality control cefpiramide raw materials.
Key words: GC; cefpiramide; residual solvent; acetone; acetonitril; N,N�dimethylformamide
Cefpiramide (cefpiramide) is the third-generation cephalosporins broad-spectrum antibiotics, can be further processed into sodium or directly for clinical, against Gram-positive bacteria, negative bacteria and anaerobic bacteria have a strong anti-bacterial viability of β � lactamase stability, a good clinical value of [1]. Since the plant produced cefpiramide using the solvent process and the use of different types of residual solvents and therefore also different, to be developed were suitable for accurate determination of the method. In this study, the Guangzhou-based pharmaceutical production Baiyunshan cefpiramide of products used in the production process to the international coordination organization (ICH) provides the second-class solvent acetonitrile and dimethylformamide, as well as three types of solvent C ketones, should be to monitor quality standards. Literature [2-3] reported similar cefpiramide sodium varieties in the determination of residual solvents, but because of the different types of residual solvents under test can not be directly quoted. In this paper, the gas chromatography, specific, able to experiment with a simultaneous determination of three kinds of solvent content, no TPD method is simple and accurate.
1 apparatus with the test drug
GC � 14A Shimadzu gas chromatograph; Dalian, according to the company produced little coating of PEG � 20M-filled glass column (3.2 mm × 2 m). Acetone and dimethyl formamide reference substance (both分析纯reagents, content 100.0%), acetonitrile reference substance (for chromatography pure reagents, content 100.0%), raw materials from cefpiramide chemical Guangzhou Baiyun Mountain pharmaceutical companies to offer high-purity nitrogen gas production from Guangzhou.
2 Methods and results
2.1 Determination of chromatographic conditions
Coating with PEG � 20M filling glass column with nitrogen as carrier gas, flow rate 10 mL / min, injection port temperature 210 ℃, and the column temperature was 100 ℃, hydrogen flame ionization detector temperature 250 ℃.
Check that n-butanol amount made by adding water to 50 μg / mL of the solution, as the internal standard solution. Said reference substance from acetone precision of about 100 mg, about 8 mg acetonitrile reference substance and reference substance dimethylformamide home about 18 mg in 100 mL量瓶, plus the internal standard solution dissolved and diluted to calibration, shake, solution as a reference substance. Precision said cefpiramide for taking samples of about 1 g, buy a plug in in vitro and accurate internal standard solution by adding 5 mL, a strong振摇5 min, filter, filtrate added check for the test materials as a solution. Precision reference substance, respectively, the volume of solution taken for the sample solution and 1 μL, into the gas chromatograph, record chromatogram using internal standard method to calculate peak area.
2.2 Chromatographic parameters, detection limit and limit of quantification
Cefpiramide sample solution for HPLC are shown in Figure 1, acetone, acetonitrile, n-butanol (internal standard) and dimethylformamide peaks were 850,800,600 column efficiency and 1 000, tailing factor 1.4,1.2,1.3 and 1.3, respectively, acetone and acetonitrile, acetonitrile and n-butanol and n-butanol and dimethylformamide peak separation between 3.9,2.8 and 7.7, respectively. Acetone, acetonitrile and dimethylformamide the detection limit (signal to noise ratio 3:1) were 1 ng, 0.5 ng and 0.5 ng, limit of quantification (signal to noise ratio 10:1) were 2 ng, 1 ng and 2 ng.
a. acetone; b. acetonitrile; c. n-butanol; d. Dimethylformamide
Figure 1 cefpiramide of residual solvents by gas chromatography (abbreviated)
Fig.1 GC Chromatograms of the residual solvents in the raw materials
Precision 2.3
Reference substance solution from sample to repeat 5 times, measured acetone, acetonitrile and dimethyl formamide and the internal standard peak area ratio of peak area RSD were 0.31%, 1.28% and 0.73%. With a homogeneous sample, in different instruments, different operators measured under the conditions of 3 results, calculated acetone, acetonitrile and dimethyl formamide content of the results of reproducibility were 1.5%, 1.9% and 1.7% respectively.
2.4 Linear relations and the scope of
Precision that were taken acetone, acetonitrile and dimethylformamide reference substance, according to "2.1" method of internal standard solution were prepared and diluted into quantitative concentration of acetone 500,750,1 000,1 500 μg / mL, acetonitrile 41,61.5,82,123,164 μg / mL and dimethylformamide 88,132,176,264,352 μg / mL of the solution, the accurate determination of 1 μL sample, the results of Jin sample volume (m) with the test solvent peak area / internal standard peak area ratio (A) of the linear regression equation are as follows: acetone A1 = 9.4826m1-0.2456 (r = 0.9997), acetonitrile A2 = 13.4495m2 +0.03646 (r = 0.9994), dimethylformamide A3 = 4.3421m3 +0.0094 (r = 0.9999); acetone, acetonitrile and dimethylformamide Determination of sample size in the range of 0.500 ~ 2.000 μg, 0.041 ~ 0.164 μg and 0.088 ~ 0.352 μg.
2.5 recovery test
According to "2.1" option, the internal standard solution were prepared with reference substance solution for the sample solution, as well as acetone, acetonitrile and dimethylformamide are equivalent to the concentration of reference substance solution of 80%, 100% and 120% of the reference substance for the test materials plus 3 copies of each solution, measured in accordance with the law injection, calculated acetone, acetonitrile and dimethylformamide of sample recovery results are as follows:
Acetone: 100.1%, 104.6%, 100.5%, 101.4%, 102.9%, 99.3%, 100.0%, 99.3% and 100.8%, with an average 101.0% (RSD 1.75%).
Acetonitrile: 97.1%, 97.5%, 96.1%, 99.8%, 96.6%, 96.3%, 99.0%, 99.2% and 97.9%, an average of 97.7% (RSD 1.40%).
Dimethylformamide: 101.2%, 99.3%, 100.8%, 102.8%, 101.4%, 99.6%, 99.3%, 98.6% and 101.0%, with an average 100.4% (RSD 1.32%).
2.6 sample
According to "2.1" Methods of determination of sample cefpiramide 3 batches get acetone content measured are as follows: 0.015%, 0.013% and 0.011%; acetonitrile content of 0.013%, 0.011% and 0.010%; dimethoxy Formamide-based content of 0.005%, 0.002%, 0.001%, are in line with the proposed limits of ICH (0.5%, 0.041% and 0.088%).
3 discussions
3.1 are three kinds of very good water-soluble solvent, cefpiramide samples by adding water to form a very strong振摇fine particles after the suspension, to ensure the dissolution of residual solvents.
Dimethylformamide 3.2 for high boiling point solvent, the aqueous solution difficult to headspace sampling method, and dimethyl formamide sample directly into a greater harm to the capillary column, thus selected column direct injection method .
3.3 Test the use of a constant column temperature measured under the conditions of stability conducive to the determination, using internal standard method helps to reduce the sampling error of operation.
Experiments show that more than 3.4, the gas chromatography specific, in the constant column temperature measured at the same time under the condition of three kinds of residual solvent content, faster and more accurate method for residual solvents cefpiramide monitoring.
【References】
[1] ZHOU Le,王明贵. Cefpiramide in vitro [J]. Chinese Journal of Antibiotics, 1997,22 (4) :275-278.
[2] Xi-Mei Wang, LI Xiao-yan, ZHOU Hai-yun, et al. Headspace Determination of sodium cefpiramide of residual solvents in the [J]. Sun Yat-sen University: Natural Science, 2004,43 (4) :122-124.
[3] Lee弘韬, Yang, Jiangling Wan, et al. Headspace solid-phase microextraction - gas chromatography cefpiramide sodium residues in a variety of organic solvents [J]. Journal of Pharmaceutical Analysis, 2005,25 (1 ) :37-39.
[4] National Pharmacopoeia Committee. People's Republic of China Pharmacopoeia: 2 [S]. Beijing: Chemical Industry Press, 2005: Appendix VE and Appendix VIII P.

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