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Article(id=1153986643288642061, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1153986642063905290, articleNumber=null, orderNo=null, doi=10.19812/j.cnki.jfsq11-5956/ts.20241018002, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1729180800000, receivedDateStr=2024-10-18, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1753061455795, onlineDateStr=2025-07-21, pubDate=1739548800000, pubDateStr=2025-02-15, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1753061455795, onlineIssueDateStr=2025-07-21, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1753061455795, creator=13701087609, updateTime=1753061455795, updator=13701087609, issue=Issue{id=1153986642063905290, tenantId=1146029695717560320, journalId=1149652044408987649, year='2025', volume='16', issue='3', pageStart='1', pageEnd='316', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=0, createTime=1753061455502, creator=13701087609, updateTime=1760070725729, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1183385652272968023, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1153986642063905290, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1183385652272968024, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1153986642063905290, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=303, endPage=308, ext={EN=ArticleExt(id=1153986643640963598, articleId=1153986643288642061, tenantId=1146029695717560320, journalId=1149652044408987649, language=EN, title=Determination of residual levels of gamithromycin in raw milk by high performance liquid chromatography-tandem mass spectrometry, columnId=1151895321388347923, journalTitle=Journal of Food Safety & Quality, columnName=Food Analysis and Detection, runingTitle=null, highlight=null, articleAbstract=

Objective To establish an analytical method for the determination of gamithromycin residues in raw milk based on matrix external standard method combined with through type purification column (EMR-Lipid) and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The samples were extracted with acid acetonitrile, purified by the EMR-Lipid through type purification column, gradient eluted through a BEH C18 chromatographic column. Detection was carried out in the electrospray positive ion multiple reaction mode, and quantification was performed using the matrix external standard method. Results Calibration curves were linear in the range of 0.5-20.0 ng/mL with correlation coefficients more than 0.99. The limit of detection (LOD) was 0.5 μg/kg, limit of quantification (LOQ) was 1.0 μg/kg. Gamithromycin showed a matrix enhancement effects in raw milk. After matrix blank curve correction, the average recoveries of gamithromycin at different spiked concentrations ranged from 74.0% to 77.0%, and the relative standard deviations (RSD) of the determination results were from 3.92% to 4.57%. Conclusion This method is accurate, sensitive, stable, simple, and easy to operate, it can be used for the rapid determination and quantitative analysis of gamithromycin residues in raw milk, providing technical support for monitoring the residual amount of gamithromycin in raw milk.

, correspAuthors=Ke-Jing LI, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, authorCompany=null, fund=null, authors=null, authorsList=Mo LI, Xin ZHAO, Hong-Ji ZHANG, Ting ZHOU, Qian WANG, Xiu-Ping ZHAO, Ke-Jing LI), CN=ArticleExt(id=1153986679024112008, articleId=1153986643288642061, tenantId=1146029695717560320, journalId=1149652044408987649, language=CN, title=高效液相色谱-串联质谱法测定生乳中加米霉素残留量, columnId=1151895321958773274, journalTitle=食品安全质量检测学报, columnName=食品分析与检测, runingTitle=null, highlight=null, articleAbstract=

目的 建立以基质外标法定量, 通过式净化柱(EMR-Lipid)结合高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)测定生乳中加米霉素残留量的分析方法。方法 样品经酸性乙腈提取后, 由EMR-Lipid通过式净化柱净化, 通过BEH C18色谱柱进行梯度洗脱, 电喷雾正离子多反应模式进行检测, 基质外标法定量。结果 加米霉素在0.5~20.0 ng/mL质量浓度范围内呈现良好线性关系, 线性相关系数大于0.99; 检出限(limit of detection, LOD)为0.5 μg/kg; 定量限(limit of quantification, LOQ)为1.0 μg/kg; 加米霉素在生乳中表现为基质增强效应, 经基质空白曲线校正后, 加米霉素在不同添加浓度平均回收率为74.0%~77.0%, 测定结果的相对标准偏差(relative standard deviation, RSD)为3.92%~4.57%。结论 该方法准确、灵敏、稳定、简单易操作, 可以用于生乳中加米霉素残留量快速测定及定量分析, 为生乳中加米霉素残留监控提供技术支持。

, correspAuthors=李克静, authorNote=null, correspAuthorsNote=
* 李克静(1981—), 女, 高级工程师, 主要研究方向为食品安全检测。E-mail:
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李默(1991—), 女, 助理研究员, 主要研究方向为农兽药残留及真菌毒素。E-mail:

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李默(1991—), 女, 助理研究员, 主要研究方向为农兽药残留及真菌毒素。E-mail:

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李默(1991—), 女, 助理研究员, 主要研究方向为农兽药残留及真菌毒素。E-mail:

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Mobile phase conditions for gradient elution

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时间
/min		 流速
/(mL/min)		 流动相A
/%		 流动相B
/%
0.00 0.400 85.0 15.0
0.50 0.400 85.0 15.0
2.80 0.400 5.0 95.0
3.50 0.400 5.0 95.0
3.60 0.400 85.0 15.0
5.00 0.400 85.0 15.0
), ArticleFig(id=1183428257132196526, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=CN, label=表1, caption=

梯度洗脱的流动相条件

, figureFileSmall=null, figureFileBig=null, tableContent=
时间
/min		 流速
/(mL/min)		 流动相A
/%		 流动相B
/%
0.00 0.400 85.0 15.0
0.50 0.400 85.0 15.0
2.80 0.400 5.0 95.0
3.50 0.400 5.0 95.0
3.60 0.400 85.0 15.0
5.00 0.400 85.0 15.0
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Mass spectrometry parameters of gamithromycin

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化合物 母离子
(m/z)		 子离子
(m/z)		 保留时间
/min		 去簇电压
/V		 碰撞能量
/V
加米霉素 777.6 619.6* 2.35 90 42
157.9 2.35 90 48
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加米霉素质谱参数

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化合物 母离子
(m/z)		 子离子
(m/z)		 保留时间
/min		 去簇电压
/V		 碰撞能量
/V
加米霉素 777.6 619.6* 2.35 90 42
157.9 2.35 90 48
), ArticleFig(id=1183428257337717425, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=EN, label=Table 3, caption=

Addition amount, recovery rate, and relative standard deviation of gamithromycin in raw milk

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化合物名称 添加量/(μg/kg) 平均回收率/% RSDs/%
加米霉素 1.0 77.0 4.57
2.0 74.0 3.92
10.0 74.9 4.51
), ArticleFig(id=1183428257392243378, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=CN, label=表3, caption=

牛乳中加米霉素的添加量、平均回收率和相对标准偏差

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化合物名称 添加量/(μg/kg) 平均回收率/% RSDs/%
加米霉素 1.0 77.0 4.57
2.0 74.0 3.92
10.0 74.9 4.51
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高效液相色谱-串联质谱法测定生乳中加米霉素残留量
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李默 , 赵鑫 , 张虹吉 , 周婷 , 王倩 , 赵修平 , 李克静 *
食品安全质量检测学报 | 食品分析与检测 2025,16(3): 303-308
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食品安全质量检测学报 | 食品分析与检测 2025, 16(3): 303-308
高效液相色谱-串联质谱法测定生乳中加米霉素残留量
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李默 , 赵鑫, 张虹吉, 周婷, 王倩, 赵修平, 李克静*
作者信息
  • 中检科(北京)测试技术有限公司, 北京 100176

    • 李默(1991—), 女, 助理研究员, 主要研究方向为农兽药残留及真菌毒素。E-mail:

通讯作者:

* 李克静(1981—), 女, 高级工程师, 主要研究方向为食品安全检测。E-mail:
Determination of residual levels of gamithromycin in raw milk by high performance liquid chromatography-tandem mass spectrometry
Mo LI , Xin ZHAO, Hong-Ji ZHANG, Ting ZHOU, Qian WANG, Xiu-Ping ZHAO, Ke-Jing LI*
Affiliations
  • Zhongjianke (Beijing) Testing Technology Co., Ltd., Beijing 100176, China
出版时间: 2025-02-15 doi: 10.19812/j.cnki.jfsq11-5956/ts.20241018002
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目的 建立以基质外标法定量, 通过式净化柱(EMR-Lipid)结合高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)测定生乳中加米霉素残留量的分析方法。方法 样品经酸性乙腈提取后, 由EMR-Lipid通过式净化柱净化, 通过BEH C18色谱柱进行梯度洗脱, 电喷雾正离子多反应模式进行检测, 基质外标法定量。结果 加米霉素在0.5~20.0 ng/mL质量浓度范围内呈现良好线性关系, 线性相关系数大于0.99; 检出限(limit of detection, LOD)为0.5 μg/kg; 定量限(limit of quantification, LOQ)为1.0 μg/kg; 加米霉素在生乳中表现为基质增强效应, 经基质空白曲线校正后, 加米霉素在不同添加浓度平均回收率为74.0%~77.0%, 测定结果的相对标准偏差(relative standard deviation, RSD)为3.92%~4.57%。结论 该方法准确、灵敏、稳定、简单易操作, 可以用于生乳中加米霉素残留量快速测定及定量分析, 为生乳中加米霉素残留监控提供技术支持。

加米霉素  /  高效液相色谱-串联质谱法  /  EMR-Lipid通过式净化柱  /  生乳

Objective To establish an analytical method for the determination of gamithromycin residues in raw milk based on matrix external standard method combined with through type purification column (EMR-Lipid) and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The samples were extracted with acid acetonitrile, purified by the EMR-Lipid through type purification column, gradient eluted through a BEH C18 chromatographic column. Detection was carried out in the electrospray positive ion multiple reaction mode, and quantification was performed using the matrix external standard method. Results Calibration curves were linear in the range of 0.5-20.0 ng/mL with correlation coefficients more than 0.99. The limit of detection (LOD) was 0.5 μg/kg, limit of quantification (LOQ) was 1.0 μg/kg. Gamithromycin showed a matrix enhancement effects in raw milk. After matrix blank curve correction, the average recoveries of gamithromycin at different spiked concentrations ranged from 74.0% to 77.0%, and the relative standard deviations (RSD) of the determination results were from 3.92% to 4.57%. Conclusion This method is accurate, sensitive, stable, simple, and easy to operate, it can be used for the rapid determination and quantitative analysis of gamithromycin residues in raw milk, providing technical support for monitoring the residual amount of gamithromycin in raw milk.

gamithromycin  /  high performance liquid chromatography-tandem mass spectrometry  /  EMR-Lipid through type purification column  /  raw milk
李默, 赵鑫, 张虹吉, 周婷, 王倩, 赵修平, 李克静. 高效液相色谱-串联质谱法测定生乳中加米霉素残留量. 食品安全质量检测学报, 2025 , 16 (3) : 303 -308 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20241018002
Mo LI, Xin ZHAO, Hong-Ji ZHANG, Ting ZHOU, Qian WANG, Xiu-Ping ZHAO, Ke-Jing LI. Determination of residual levels of gamithromycin in raw milk by high performance liquid chromatography-tandem mass spectrometry[J]. Journal of Food Safety & Quality, 2025 , 16 (3) : 303 -308 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20241018002
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0 引言
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加米霉素(gamithromycin)是一种新型的半合成大环内酯类兽用抗生素, 由法国梅里亚公司研发, 其结构式如图1所示。该药的杀菌作用是通过抑制敏感菌RNA依赖性蛋白合成来实现的, 常用于兽医临床因巴氏杆菌、支原体、睡眠嗜组织菌等感染所致的牛呼吸系统疾病(bovine respiratory disease, BRD)的治疗[1-3]。是我国批准的用于治疗牛、猪部分呼吸道疾病的二类新兽药[4]。
作为新一代大环类脂类抗菌药的加米霉素, 具备给药吸收快、抗菌活性强、肺部药物浓度高、毒性低以及组织残留少等优点, 拥有广阔的临床应用前景[5-6]。欧洲药品局(European Medicines Agency, EMA)先后在2007年和2016年将加米霉素批准用于靶动物牛和猪[7-9]; 2010年, 加拿大保健产品与食品管理局(Health Products and Food Administration of Canada, HPFB)批准加米霉素用于防止溶血性曼氏杆菌等引起的BRD; 2011年, 美国食品与药品管理局(US Food and Drug Administration, FDA)也批准了该药用于此用途[10-13]。依据我国相关规定, 加米霉素只在猪、牛的肌肉、肝、肾等靶组织中有相关的最大残留限量要求, 并未对生乳及牛奶中加米霉素的残留限量进行规定, 但是欧盟在EU No 470/2009中规定加米霉素在泌乳期禁用。生乳的质量安全一直是社会各界关注的重点, 建立生乳中加米霉素稳定、快速、灵敏的检测方法对保证我国奶源安全及出口乳品的质量, 了解加米霉素的污染情况具有实际意义。
目前, 加米霉素的分析方法主要是高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)[14-17]。样品基质多为猪、牛的肌肉组织。乳制品基质检测, 目前在国内偶见报道。烟利亚[14]建立了利用液相色谱-串联质谱法测定猪肉和牛肉中双氯酚酸、氟尼辛、加米霉素的残留量; 王艳艳等[15]通过液相色谱串联-质谱仪对牛可食性组织中加米霉素残留量进行测定; 虽然陈心怡等[17]建立了液相色谱-串联质谱法测定牛奶中加米霉素的分析方法, 但是该方法使用同位素内标定量, 相较而言成本较高, 不便于推广。近年来, 通过式固相萃取技术作为一种新型的前处理净化方式以成本低, 操作简单, 耗时短等优势被广泛应用于食品检测中[18-24]。本研究以基质空白曲线定量, 通过式净化柱(EMR-Lipid)结合HPLC-MS/MS建立起一种前处理方法简单、成本较低、易于推广的加米霉素的分析方法, 以满足日常生乳中加米霉素的监控需求。
1 材料与方法
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1.1 材料与试剂
乙腈(色谱纯, 上海安谱公司); 甲酸(优级纯, 北京百灵威科技有限公司); 乙酸铵(色谱纯, 美国Sigma公司); 加米霉素标准溶液(质量浓度100 μg/mL, 天津阿尔塔First Standard公司)。
1.2 仪器与设备
岛津LC-30A高效液相色谱仪(日本岛津公司); Triple Quad 4500三重四极杆质谱仪(美国AB公司); ACQUITY UPLC BEH C18色谱柱(100 mm×2.1 mm, 1.7 μm, 美国Waters公司); SR-2DS振荡器(日本TAITEC公司); ME203E分析天平(精度10 mg)、ME204E分析天平(精度0.1 mg)[梅特勒托利多科技(中国)有限公司]; X-15R离心机(德国Beckman公司); Milli-Q EQ7008超纯水机(美国Millipore公司); SI Vortex Genie 2漩涡混合器(美国Scientific Industries公司); Captuve EMR-Lipid净化柱(300 mg/3 mL, 美国安捷伦公司); 0.22 μm有机相滤膜(天津津腾实验设备有限公司)。
1.3 试验方法
1.3.1 标准溶液配制
准确吸取适量的加米霉素标准品, 用乙腈稀释混匀, 定容至10 mL, 得到10 μg/mL标准储备溶液, 置于-18 ℃冰箱保存。取适量该溶液, 分别配制0.20 μg/mL和0.02 μg/mL的标准工作溶液。精密吸取标准工作液适量, 用经提取净化后的空白样品溶液稀释配制成0.5~20.0 ng/mL的系列基质校准工作曲线。
1.3.2 样品前处理
称取生乳5 g(精确至0.01 g)置于50 mL离心管中, 加入0.2%甲酸-乙腈溶液定容至15 mL, 振荡20 min, 8000 r/min离心5 min, 上清液转移至另一套离心管中, 待净化。
取3 mL上清液过EMR-Lipid通过式净化柱(无需活化), 上样后立即接收。待样液全部流完之后, 再加入1 mL 0.2%甲酸-乙腈溶液淋洗小柱并合并样液, 抽干小柱。将收集的过柱液体在40 ℃下用氮气吹至近干, 加入0.5 mL 0.05%甲酸-乙酸铵溶液, 用乙腈定容至1 mL, 涡旋混合均匀, 过0.22 μm滤膜, 供HPLC-MS/MS分析。
1.3.3 液相色谱-串联质谱条件
(1)液相色谱条件
色谱柱为ACQUITY UPLC BEH C18 (100 mm×2.1 mm, 1.7 μm, 美国Waters公司); 流动相A: 水(含0.1%甲酸), 流动相B: 乙腈; 流速: 0.4 mL/min; 进样量: 6.00 µL; 柱温: 45 ℃; 洗脱的梯度条件如表1所示。
(2)质谱条件
电离源: 电喷雾正离子模式(electrospray ionization, ESI+); 监测模式: 多反应监测(multiple reaction monitoring, MRM); 气帘气: 35 psi; 雾化气: 氮气, 50 psi; 辅助加热气: 氮气, 55 psi; 碰撞气: 氮气; 离子喷雾电压: 5500 V; 辅助加热器温度: 500 ℃; 加米霉素质谱参数如表2所示。
1.4 数据处理
方法学验证参照GB 5009.295《食品安全国家标准 化学分析方法验证通则》进行分析验证。在方法学考察中, 重复性实验平行测定大于6次, 回收率测定3组7份, 线性测定5个点(不包括零点), 每个点测定3份, 实际样品平行测定3份, 数据采集和分析软件分别为Analyst 1.6版本、Analyst 1.6.3系统软件和Excel 2016, 结果以平均数表示。
2 结果与分析
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2.1 前处理条件优化
2.1.1 提取溶剂优化
乙腈、甲醇、甲酸乙腈以及磷酸盐缓冲溶液是常用的加米霉素提取溶剂。由于EMR-Lipid通过式净化柱是利用极性、非极性及离子交换等基团组成的填充剂进行选择性的吸附而达到去除样品干扰物的目的, 若选择磷酸盐缓冲液则会明显干扰净化效果, 故不将其作为本研究的提取溶液。用甲醇进行提取时, 由于乳化现象较严重, 因此也不作为最佳的提取溶剂; 本研究对乙腈、2.0%甲酸-乙腈、1.0%甲酸-乙腈、0.5%甲酸-乙腈、0.2%甲酸-乙腈和0.1%甲酸-乙腈6种提取溶剂的提取效率进行了对比。具体回收率的结果比较见图2。结果表明: 6种提取溶剂中, 乙腈的回收率在5.0%左右, 0.1%甲酸-乙腈的回收率在65%左右, 0.2%、0.5%、1.0%、2.0%甲酸-乙腈的回收率分别为: 82.0%、79.4%、81.6%、79.8%。综合考虑测试成本因素, 最终选用0.2%甲酸-乙腈作为本研究的提取溶剂。
2.1.2 净化方式优化
本研究采用EMR-Lipid通过式净化柱净化, 无需活化, 且上样后直接接收, 净化液直接进行氮吹浓缩、过膜后供仪器分析测试。结果表明: (1)在相应的保留时间处, 空白基质样品对被测物无显著干扰; (2)所得到的加米霉素回收率处于60%~120%的范围之内, 满足GB 5009.295《食品安全国家标准 化学分析方法验证通则》的要求, 同时还能够极大地提高测试效率。故本研究采用EMR-Lipid通过式净化柱进行净化。
2.1.3 基质效应的评估
采用液相色谱-串联质谱法测定时, 基质效应会对分析结果产生影响[25-28]。根据MATUSZEWSKI等[29]的方法, 基质效应=(基质匹配标准曲线斜率-溶剂标准曲线斜率)/溶剂标准曲线斜率×100%。若结果为负数则表示基质抑制效应, 结果为正数表示基质增强效应。当-20%<基质效应<20%之间时为弱基质效应; 如果在-50%<基质效应<20%或20%<基质效应<50%之间, 则为中等基质效应; 基质效应≥50%或基质效应≤50%时为强基质效应[30]。
按1.3的试验方法配制基质匹配标准曲线和溶剂标准曲线。溶剂标准曲线线线性方程: Y=20793.90478X- 1506.77265 (r2=0.99953), 基质匹配曲线线性方程为: Y=29847.58152X-1943.54824 (r2=0.99819)。结果表明加米霉素在生乳基质中的基质效应为43.5%, 表明存在中等基质增强效应。所以, 为抵消基质效应的影响, 选择基质匹配标准曲线来进行定量。
2.2 质谱条件优化
加米霉素含有羧基, 易结合氢离子[31], 本研究通过流动注射进样方式选择并优化MRM参数, 在正离子模式下选择[M+H]+为母离子, 优化碰撞能量以获得响应较高的子离子。把丰度最强的离子对作为定量离子对, 接着对毛细管电压、雾化气流速、锥孔气流速、雾化气温度、源温度、锥孔电压、碰撞能量等质谱条件予以优化, 最终确定的质谱条件如表2所示。按照上述色谱和质谱条件获得的标准溶液图谱详见图3。
2.3 方法学验证
2.3.1 线性范围
按照1.3.1所述采用空白生乳基质标准工作液, 配制成加米霉素质量浓度为0、0.5、1.0、2.0、5.0、10.0、20.0 ng/mL的系列基质匹配标准工作液, 供HPLC-MS/MS检测。采用MRM离子扫描方式, 将定量离子对峰面积作为纵坐标, 把基质标准溶液浓度当作横坐标, 拟合出基质校准标准曲线。考察加米霉素在0.5~20.0 ng/mL的质量浓度范围内线性方程及其相关系数。结果表明, 在0.5~20.0 ng/mL质量浓度范围内呈现良好的线性关系, 线性方程为Y=29847.58152X-1943.54824(相关系数r=0.999)。
2.3.2 检测方法灵敏度
在生乳空白基质样品中添加一定浓度的加米霉素平行测定10次, 当检出率大于50%, 且有检出的信噪比(S/N)均大于等于3时, 将其确定为检出限(limit of detection, LOD), 相关图谱见图4。结果表明10次测定的检出率为100%, 并且有检出的信噪比(S/N)均大于等于3, 该方法下加米霉素的检出限为0.5 μg/kg, 满足GB 5009.295的要求。
在生乳空白基质样品中添加一定浓度的加米霉素平行测定7次, 且信噪比(S/N)均大于等于10为定量限(limit of quantification, LOQ), 图谱见图5。结果表明7次测定的信噪比(S/N)均大于等于10, 该方法下加米霉素的LOQ为1.0 μg/kg, 满足GB 5009.295的要求。
2.3.3 检测方法的精密度和准确度
选取牛乳空白基质样品, 开展添加回收和精密度试验。进行3水平添加试验时, 选取方法LOQ、2倍方法LOQ和10倍方法LOQ, 每个水平平行测定7次, 并且进行重复性验证, 结果详见表3, 添加样品图谱见图6、图7。结果表明加米霉素在不同添加浓度的平均回收率为74.0%~77.0%之间, 测定结果的RSDs为3.92%~4.57%之间。该加标水平下, 精密度良好, 回收率满足GB 5009.295的要求。
2.4 实际样品检测
对200个生乳样品进行加米霉素测定, 检测方法按照本研究所述开展, 均未检测出加米霉素。
3 结论
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本研究建立了一种采用HPLC-MS/MS检测生乳中加米霉素的测定方法。该方法以酸性乙腈作为提取溶剂, 经EMR-Lipid通过式净化柱净化后, 进行氮吹浓缩复溶以供HPLC-MS/MS测定。其具有干扰小、提取效率高、分析时间快等优点。通过添加空白样品的回收实验测定, 证实此方法灵敏度好、准确度高、稳定性好且简单易操作, 适用于生乳中加米霉素的定性定量分析。
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2025年第16卷第3期
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doi: 10.19812/j.cnki.jfsq11-5956/ts.20241018002
  • 接收时间：2024-10-18
  • 首发时间：2025-07-21
  • 出版时间：2025-02-15
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  • 收稿日期：2024-10-18
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    中检科(北京)测试技术有限公司, 北京 100176

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* 李克静(1981—), 女, 高级工程师, 主要研究方向为食品安全检测。E-mail:
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2种不同金属材料的力学参数
科
Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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