Page 11 - Clinical-Medical Solution for Clinical Chemistry
P. 11
Application No. C153
News
Table 4 Quantitative Results of the Table 5 Quantitative Results of the
Manual Pretreatment Method and Manual Pretreatment Method and
Fully Automated Pretreatment Analysis Method Fully Automated Pretreatment Analysis Method
(Amiodarone) (Desethylamiodarone)
Amiodarone Desethylamiodarone
Manual Automated Manual Automated Ratio %*
[ng/mL] [ng/mL] Ratio %* [ng/mL] [ng/mL]
Sample 1 373 411 110.2 Sample 1 304 271 89.1
Sample 2 399 404 101.3 Sample 2 412 366 88.8
Sample 3 546 557 102.0 Sample 3 416 423 101.7
Sample 4 205 211 102.9 Sample 4 271 240 88.6
Sample 5 963 895 92.9 Sample 5 717 654 91.2
Sample 6 1,318 1,213 92.0 Sample 6 151 150 99.3
Sample 7 1,271 1,229 96.7 Sample 7 431 408 94.7
Sample 8 1,233 1,282 104.0 Sample 8 664 628 94.6
Sample 9 2,259 2,208 97.7 Sample 9 940 1,080 114.9
Average 100.0 Average 95.9
RSD % 5.8 RSD % 8.9
* Automated Pretreatment / Manual Pretreatment * Automated Pretreatment / Manual Pretreatment
AMD DEA
2500 R² = 0.9946 1250 R² = 0.9541
y = 1.007x
y = 0.975x
Automated Pretreatment [ng/mL] 1500 Automated Pretreatment [ng/mL] 750
2000
1000
500
1000
500
250
0
500
750
500
0
1000
1500
Manual Pretreatment 2000 2500 0 0 250 Manual Pretreatment 1000 1250
[ng/mL] [ng/mL]
Comparison of Quantitative Results for Amiodarone Comparison of Quantitative Results
for Desethylamiodarone
Table 6 Analysis Conditions (Comparative Test of Pretreatment Methods)
System : CLAM-2000 + Nexera + LCMS-8040
Protocol : Plasma disp. 50 μL - acetonitrile disp. 225 μL - mixing at 1900 rpm, 120 sec - filtration for 90 sec
Column : Shimadzu GLC Mastro C18 (50 mmL. × 2.1 mmI.D., 3 μm)
Mobile Phase : A) 0.1% Formic acid - Water, B) 0.1% Formic acid - Methanol
Flow Rate : 0.4 mL/min
Time program : B Conc. 10 % (0 min) – 100 % (2 – 3.5 min) – 10 % (3.51 – 6 min)
Column Temp. 50 °C Injection Volume : 0.1 μL
Probe Voltage : 4.5 kV (ESI-positive mode)
DL Temp. : 250 °C Block Heater Temp. : 400 °C
Neb. Gas Flow : 3 L/min Drying Gas Flow : 15 L/min
[Acknowledgments]
We would like to thank pharmacist Yuko Shimamoto of the Pharmacy Division at the National Cerebral and Cardiovascular Center Hospital
(National Research and Development Agency) in Japan for her significant cooperation in the investigation provided in this article.
References • Guidance for Industry : Bioanalytical Method Validation (2001, US FDA)
• Guideline on Bioanalytical Method Validation in Pharmaceutical Development (2013, Japan MHLW)
Notes • The product described in this document has not been approved or certified as a medical device under the Pharmaceutical and
Medical Device Act of Japan. It cannot be used for the purpose of medical examination and treatment or related procedures.
• The samples described in this document were all sampled and measured at the National Cerebral and Cardiovascular Center
Hospital in Japan. Permission was obtained regarding the publication of measurement data.
First Edition: Aug. 2017
For Research Use Only. Not for use in diagnostic procedure.
This publication may contain references to products that are not available in your country. Please contact us to check the availability of these
products in your country.
The content of this publication shall not be reproduced, altered or sold for any commercial purpose without the written approval of Shimadzu.
Company names, product/service names and logos used in this publication are trademarks and trade names of Shimadzu Corporation or its
affiliates, whether or not they are used with trademark symbol “TM” or “£”. Third-party trademarks and trade names may be used in this
publication to refer to either the entities or their products/services. Shimadzu disclaims any proprietary interest in trademarks and trade names
www.shimadzu.com/an/ other than its own.
The information contained herein is provided to you "as is" without warranty of any kind including without limitation warranties as to its
accuracy or completeness. Shimadzu does not assume any responsibility or liability for any damage, whether direct or indirect, relating to the
use of this publication. This publication is based upon the information available to Shimadzu on or before the date of publication, and subject
to change without notice.
© Shimadzu Corporation, 2017